Document LJ8rLdRmqewGKmz3ZbdDw8gdQ

N36678 DUP050297150 Louviers Library n ? * DUP050297151 I` A 01 m? DUP050297152 1992 Cl ANNUAL BOOK E M /1STM SMND^RDS Paints, Related Coatings, and Aromatics VOLUME Paint--Tests for Formulated Products 06.01 and Applied Coatings Includes standards of the following committee: D-1 on Paint and Related Coatings and Materials D-33 on Protective Coating and Lining Work for Power Generation Facilities Publication Code Number (PCN): 01-060132-14 , ASTM 1916 Race Street, Philadelphia, PA 19103-1187 USA (215)299-5400 TWX: 710-670-1037 FAX: 215-977-9679 DUP050297153 Director, Editorial Services: Roberta A. Storer Manager, Standards Publications: Joan L. Comillot Susan P. Milligan Senior Indexer: H. Joel Shupak Editorial Staff Editors: Paula C. Fazio Donna Fisher . ' Elizabeth L. Gutman Catherine T. Hsia Sharon L. Kauffman Joanne Kramer Marianne Lane Christine M. Leinweber Vemice A. Mayer Patricia A. McGee Editorial Assistants: Todd J. Sandler Mariano J. Sikora Richard F. Wilhelm library of Congress Catalog Card Number: 83-641658 ISBN 0-8031-1754-x (set) ISBN 0-8031-1706-x (section) ISBN 0-8031-1707-8 (volume) Copyright 1992 AMERICAN SOCIETY FOR TESTING AND MATERIALS, Philadelphia, PA. Prior editions copyrighted 1991 and earlier, by the American Society for Testing and Materials. All rights reserved. This material may not be reproduced or copied, in whole or in part, in any printed, mechanical, electronic, film, or other distribution and storage media, without the written consent ofthe publisher. Photocopy Rights Authorization to photocopy items for internal or personal use, or the internal or personal use of specific clients, is granted by the AMERICAN SOCIETY FOR TESTING AND MATERIALS for users registered with the Copyright Clearance Center (CCC) Transactional Reporting Service, provided that the base fee of $2.50 per copy, plus $0.50 per page is paid directly to CCC, 27 Congress St., Salem, MA 01970; Tel. (508) 744-3350. 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V DUP050297157 ANNUAL BOOK OF ASTM STANDARDS Listed by Section and Volume Section 1--Iron and Steel Products Volume 01.01 Steel--Piping, Tubing, Fittings Volume 01.02 Ferrous Castings; Ferroalloys Volume 01.03 Steel--Plate, Sheet, Strip, Wire Volume 01.04 Steel--Structural, Reinforcing, Pressure Vessel, Railway Volume 01.05 Steel--Bars, Forgings, Bearing, Chain, Springs Volume 01.06 Coated Steel Products Volume 01.07 Shipbuilding Section 2--Nonferrous Metal Products Volume 02.01 Copper and Copper Alloys Volume 02.02 Aluminum and Magnesium Alloys Volume 02.03 Electrical Conductors Volume 02.04 Nonferrous Metals--Nickel, Cobalt, Lead, Tin, Zinc, Cadmium, Precious, Reactive, Refractory Metals and Alloys Volume 02.05 Metallic and Inorganic Coatings; Metal Powders, Sintered P/M Structural Parts Section 3--Metals Test Methods and Analytical Procedures Volume 03.01 Metals--Mechanical Testing; Elevated and Low-Temperature Tests; Metallography Volume 03.02 Wear and Erosion; Metal Corrosion Volume 03.03 Nondestructive Testing Volume 03.04 Magnetic Properties; Metallic Materials for Thermostats, Electrical Heating and Resistance, Contacts, and Connectors Volume 03.05 Analytical Chemistry for Metals, Ores, and Related Materials (I): A 751 to E 354 Volume 03.06 Analytical Chemistry for Metals, Ores, and Related Materials (II):E 356 to latest; Surface Analysis Section 4--Construction Volume 04.01 Cement; Lime; Gypsum Volume 04.02 Concrete and Aggregates Volume 04.03 Road and Paving Materials; Pavement Management Technologies Volume 04.04 Roofing, Waterproofing, and Bituminous Materials Volume 04.05 Chemical-Resistant Materials; Vitrified Clay, Concrete, Fiber-Cement Products; Mortars; Masonry Volume 04.06 Thermal Insulation; Environmental Acoustics Volume 04.07 Building Seals and Sealants; Fire Standards; Building Constructions Volume 04.08 Soil and RockfDimension Stone; Geosynthetics Volume 04.09 Wood Section S--Petroleum Products, Lubricants, and Fossil Fuels Volume 05.01 Petroleum Products and Lubricants (I): D 56-D 1947 Volume 05.02 Petroleum Products and Lubricants (II): D 1949-D 3601 Volume 05.03 Petroleum Products and Lubricants (III): D 3602-latest; Catalysts Volume 05.04 Test Methods for Rating Motor, Diesel, and Aviation Fuels Volume 05.05 Gaseous Fuels; Coal and Coke Section 6--Paints, Related Coatings, and Aromatics Volume 06.01 Paint--Tests for Formulated Products and Applied Coatings Volume 06.02 Paint--Pigments, Resins, and Polymers; Cellulose Volume 06.03 Paint--Fatty Oils and Acids, Solvents, Miscellaneous; Aromatic Hydrocarbons DUP050297158 LISTED BY SECTION AND VOLUME Section 7--Textiles Volume 07.01 Textiles (I): D 76-D 3219 Volume 07.02 Textiles (II): D 3333-latest Section 8--Plastics Volume 08.01 Plastics (I): C 177-D 1600 Volume 08.02 Plastics (II): D 1601-D 3099 Volume 08.03 Plastics (III): D 3100-latest Volume 08.04 Plastic Pipe and Building Products Section 9--Rubber Volume 09.01 Rubber, Natural and Synthetic--General Test Methods; Carbon Black Volume 09.02 Rubber Products, Industrial--Specifications and Related Test Methods; Gaskets; Tires Section 10--Electrical Insulation and Electronics Volume 10.01 Electrical Insulation (I)--D 69-D 2484 Volume 10.02 Electrical Insulation (II)--D 2518-latest Volume 10.03 Electrical Insulating Liquids and Gases; Electrical Protective Equipment Volume 10.04 Electronics (I) Volume 10.05 Electronics (II) Section 11--Water and Environmental Technology Volume 11.01 Water (I) Volume 11.02 Water (II) Volume 11.03 Atmospheric Analysis; Occupational Health and Safety Volume 11.04 Pesticides; Resource Recovery; Hazardous Substances and Oil Spill Responses; Waste Management; Biological Effects Section 12--Nuclear, Solar, and Geothermal Energy Volume 12.01 Nuclear Energy (I) Volume 12.02 Nuclear (II), Solar, and Geothermal Energy Section 13--Medical Devices and Services Volume 13.01 Medical Devices; Emergency Medical Services Section 14--General Methods and Instrumentation Volume 14.01 Analytical Methods--Spectroscopy; Chromatography; Computerized Systems Volume 14.02 General Test Methods, Nonmetal; Laboratory Apparatus; Statistical Methods; Appearance of Materials; Durability of Nonmetallic Materials Volume 14.03 Temperature Measurement Section 15--General Products, Chemical Specialties, and End Use Products Volume 15.01 Refractories; Carbon and Graphite Products; Activated Carbon Volume 15.02 Glass; Ceramic Whitewares Volume 15.03 Space Simulation; Aerospace and Aircraft; High Modulus Fibers and Composites Volume 15.04 Soap; Polishes; Leather, Resilient Floor Coverings Volume 15.05 Engine Coolants; Halogenated Organic Solvents; Industrial Chemicals Volume 15.06 Adhesives Volume 15.07 End Use Products Volume 15.08 Fasteners Volume 15.09 Paper, Packaging; Flexible Barrier Materials; Business Imaging Products Section 00--Index Volume 00.01 Subject Index and Alphanumeric List vii DUP050297159 ANNUAL BOOK OF ASTM STANDARDS Listed by Subjects SUBJECT VOLUME SUBJECT VOLt) Acoustics, Environmental.............................................. Activated Carbon.............................................................. Adhesives........................................................................... Advanced Ceramics......................................................... Aerosols.............................................................................. 04.06 15.01 15.06 15.01 15.09 Glass. Shipping........................................................................ Coolants, Engine............................................................ Copper and Copper Alloys........... ............................ [ Corrosion, Metal ..................................................... ' 1ls5] jjjjp 031 Aerospace Industry Methods......................................... 15.03 Criteria for the Evaluation of Testing and Inspection Aggregates................ ....................................................... 04.02 Aluminum and Aluminum Alloys.............................. 02.02 Agencies.......................... ..................................... 141 Detention and Correctional Facilities........................ Q41 Amusement Rides and Devices.................................. 15.07 Analytical Atomic Spectroscopy....................... 03.05, 03.06 Anesthetic and Respiratory Equipment..................... 13.01 Appearance of Materials................................................ 14.02 Aromatic Hydrocarbons and Related Die-Cast Metals.................. ............. .............................. Dimension Stone............................................................ Dosimetry ........................................................................ Ductile Iron..................................................................... Durability of Nonmetallic Materials....... ............... Q2J Q044.10ft 123 oij 14*1 Chemicals.............................................................. 06.03 Electrical Conductors ................................................... 02J Atmospheric Analysis..................................................... 11.03 Electrical Contacts and Connectors .......................... ojj Biological Effects and Environmental Fate............................. 11.04Electrical Insulating Materials......... ................. 10.01, 10.1 Biotechnology.................................................................. 11.04 . i6.o| Bituminous Materials..................................................... 04.03 Electrical Protective Equipment for Workers........... I0 `f|; Building Constructions................................................... Building Seals and Sealants............................................ Business Imaging Products........................................... Carbon Black..................................................................... 04.07 04.07 15.09 09.01 Electronics......................... ..................................... 10.04, Emergency Medical Services....................................... lj.j) Emission Spectroscopy........................................ 03.05* 03,,0 Erosion and Wear................................ ...................... fgjj| Carbon Products, Manufactured.................................. Cast Iron ............................................................................ Catalysts.............................................................................. 15.01 01.02 05.03 Evaluating Testing and Inspection Agencies........... Exposure .Tests............ .................................................... Fasteners ................................................ ......................... 14.0 144 15.1 Cellulose.............................................................................. 06.02 Fatigue ............................................................................... 03.01 Cement................................................................................ Hydraulic....................................................................... Rubber........................................................................... Ceramic Materials....... .................................................... Advanced Ceramics..................................................... Ceramic Whitewares.................................................. 04.01 04.01 09.01 15.02 15.01 15.02 Fences.............................................................................. 01.06, Ferroalloys..........................................--...................... 01.02 -j Ferrous Castings ............................. .............................. 01.02^ .Fiber-Cement Products......................................... 04.0S ^ Filtration ...................................................................... 14.02 Fire Standards......................... .......................... ,. >.. ..;:.0407 Ceramics for Electronics....... ........................... 10.04 Flexible Barrier Materials.................... ............... .... .15.09 Porcelain Enamel......................................................... 02.05 Food-Service Equipment................s............................^ 15.07 Chemical Analysis of Metals........... .................. 03.05, 03.06 Footwear, Safety and Traction for .............. 15.07 Chemical-Resistant Nonmetallic Materials.............. 04.05 Forensic Sciences..................................................... 13.01 Chemicals, Industrial....................................................... 15.05 Fracture Testing.................................... -...................... 03.()1 Chromatography.............................................................. 14.01 Gaseous Fuels........................................ ...............-- 0545 Closures.............................................................................. 15.09 Coal and Coke................................................................... 05.05 Gaskets...... .............................................................;----- 09.02 Geotextiles and Related Products............. ................. 04.08 Compatibility and Sensitivity of Materials in Oxy Geothermal Resources and Energy............. .................... 12:02 gen-Enriched Atmospheres.............................. 14.02 Glass............................... .,15.02 Computerization of Material Property Data...........................14.01Graphite Products, Manufactured ............................. 15-01 Computerized Systems.................................................. 14.01 Graphite Products, Nuclear ........................................ 52.02 Concrete and Concrete Aggregates.............................. 04.02 Gypsum............................................................................ J.01 Concrete Pipe and Tile................................................... 04.05 Halogenated Organic Solvents .................................... *5.05 Concrete Products, Precast............................................ 04.05 Hazardous Substances and Oil Spill Response----- 11.04 Concrete Reinforcing Steel............................................ 01.04 Hazard Potential of Chemicals................................... J4.02 Consumer Products......................................................... 15.07 Health Care Services and Equipment........................ J3.01 Containers: High Modulus Fibers and Composites...................... J5-03 Aerosol............................................................................ 15.09 Imaging Products, Business............................. i5-W via DUP050297160 LISTED BY SUBJECTS SUBJECT VOLUME SUBJECT VOLUME Index (for all volumes).................................................. 00.01 Refractories....................................................................... 15.01 Industrial Chemicals....................................................... 15.05 Resilient Floor Coverings............................................. 15.04 Iron Castings..................................................................... 01.02 Resinography.................................................................... 14.01 Knock Test Manual ....................................................... 05.04 Resource Recovery ....:............................................. 11.04 Laboratory Apparatus..................................................... 14.02 Road and Paving Materials........................................... 04.03 Leather................................................................ 15.04 Robotics.............................................................. 14.01 Lime.................................................................................... 04.01 Roofing, Waterproofing, and Bituminous Magnesium and Magnesium Alloys........................... 02.02 Materials............................................................. 04.04 Magnetic Properties......................................................... 03.04 Rubber....................................................................... 09.01,09.02 ME Malleable Iron ................................................................. 01.02 Security Systems and Equipment................................ 15.07 .02 Masonry Units.................................................................. 04.05 Sensory Evaluation of Materials and Products .... 15.07 .09 Meat and Poultry............................................... 15.07 Shipbuilding....................................................................... 01.07 .05 Medical and Surgical Materials and Devices......... 13.01 Sintered P/M Structural Parts....................................... 02.05 .01 Metallic and Inorganic Coatings................................ ^ 02.05 Skiing, Snow...................... 15.07 02 Metallography...................... 03.01 Soap.................................................................................... 15.04 Metal Powders.................................................................. 02.05 Soil and Rock.................................................................. 04.08 02 Metals, Chemical Analysis.................................. 03.05,03.06 Solar Energy Conversion................................................ 12.02 07 Metals, Effect of Temperature on Properties-------- 03.01 Space Simulation.............................................................. 15.03 04 Metals, Physical and Mechanical Testing.. ............ 03.01 Spectroscopy........................................................... 03.06, 14.01 08 Metric Practice..............................................................^. 14.02 Sports Equipment and Facilities............................. 15.07 02 Mortars for Unit Masonry ............................................ 04.05 Statistical Methods ......................................................... 14.02 02 Naval Stores......................................... 06,03 Steel: 02 Nickel and Nickel Alloys .............................................. 02.04 Bars ............................................................................... 01.05 03 Nondestructive Testing.................................. 03.03 Bearing Steel............................................................... 01.05 04 Nonferrous Metals, General......................................... 02.04 Bolting.....................................................................01.01, 15.08 >2, Nonmetals, General Test Methods.............................. 14.02 Castings........................................................................ 01.02 03 Nuclear Materials................................................ 12.01, 12.02 Chain............................................................................. 01.05 33 Occupational Health and Safety.................................. 11.03 Concrete Reinforcing.:......................................... 01.04 35 Oil Spill Response, Hazardous Substances................ 11.04 Detention and Correctional Facilities.................... 04.07 31 Ores, Metal Bearing, Sampling and Analysis . 03.05, 03.06 Fasteners........................ 15.08 36 Orthotics, External Prosthetics, and Mobility Forgings................................................................ 01.04,01.05 32 Aids........................................................................ ` 13.01 Galvanized.................................................................... 01.06 32 Packaging............................................. 15.09 Piping, Tubing, and Fittings.................................... 01.01 32 Paint and Related Coatings and Materials: Plate, Sheet, and Strip................................................ 01.03 >8 Fatty Oils and Acids, Solvents, Miscellaneous... 06.03 Pressure Vessel Plate and Forgings......................... 01.04 (1 Pigments, Resins, and Polymers.............................. 06.02 Rails, Wheels, and Tires........................................... 01.04 >6 Tests for Formulated Products and Applied Coat Springs........................................................................... 01.05 32 ings ...................................................................... 06.01 Stainless Steel................................................................ 01.01, >2 Paper................................................................................... 15.09 01.02,01.03,01.04,01.05 Pavement Management Technologies....................... 04.03 Structural Steel ........................................................... 01.04 Particle Size Measurement............................. 14.02 Wire......... -.................................................................... 01.03 Pesticides............................. 11.04 Surface Analysis................................................................ 03.06 Petroleum Products and Lubricants............................ 05.01, Surgical Materials and Devices.................................... 13.01 05.02, 05.03, 05.04 Temperature Measurement........................................... 14.03 Plastics.................................. 08.01, Textiles......................................... 07.01,07.02 08.02,08.03 Thermal Measurements.............. ................................... 14.02 1 Plastic Pipe and Building Products.............................. 08.04 Thermal Insulation......................................................... 04.06 5 Polishes ........................................... 15.04 Thermocouples............................................................... 14.03 2 Porcelain Enamel.............................................................. 02.05 ; Thermostats, Electrical Heating and Resistance, 8 Pressure Vessel Plate and Forgings.............................. 01.04 Contacts, and Connectors................................ 03.04 2 Products Liability Litigation, Technical Aspects Tires.................. 09.02 2 of..................................................................... 14.02 Traveled Surface Characteristics.................................. 04.03 1 Protective Clothing....................................... '.15107 Vacuum Cleaners ............................. 15.07 2 Protective Coating and Lining Work for Power Vitrified Clay Pipe............................................... 04.05 1 Generation Facilities................................ 06.01, 12.01 Waste Management.................................. ...................... 11.04 5 Protective Equipment, Electrical, for Workers......... 10.03 Water................................................. 11.01,11.02 4 Radioisotopes and Radiation Effects............... ' 12.02 Wear and Erosion........................................................... 03.02 2 Reactive and Refractory Metals................................... 02.04 Wood....... ........................................................................... 04.09 I 3 ix- DUP050297161 Contents 1992 ANNUAL BOOK OF ASTM STANDARDS, Volumes 06.01, 06.02, and 06.03 S " " R' G < { t o P < -T' E F9 #G ' " P"( t s " &&A G < ' " C !< { "; P< { $9 ' t s , R' %< '% ( " P)G 09 ' 1s ; 2 34C' G G G ' ; F 556 7 8O< G " 9 @ A BC@ DE FA , M( < " < ( 'GG ' ; A 9 <( HG"HI( H ' In s A complete Subject Index begins on p. 1133 This contents includes only those standards included in these books and those standards that appeared previously that have been superceded or discontinued within the past five'years. Since the standards in these books are arranged in alphanumerical sequence, no page numbets are given in this contents. The alphanumerical sequence in Volume 06.03 is divided into two sections, separating the standards of Committee D-l and D-16. In the serial designations prefixed to the following titles, the number following the dash indicates the year of original adoption as standard or, in the case bf revision, the year of last revision. Thus, standards adopted or revised during the year 1992 have as their final number, 92. A letter following' this number indicates more than one revision during that year, that is 92a indicates the second revision in 1992, 92b the third revision, etc. Standards that have been reapproved without change are indicated by the year of last reapprovai in parentheses as part of the designation number, for example, (1992). A superscript epsilon indicates an editorial change since the last revision or reapproval--el for the first change, e2 for the second change, etc. PAINT AND RELATED COATINGS AND MATERIALS B 117-90 B 287 -74(1980)" D 12-88 D 13-82(1987) D 16-91 D 29-81 (1987)" D 34-91 D 49-83(1990)" D 50-90 D 56-87 D 79-86 D 81-87 D 83-84(1989) D 85-87(1991)" D 86-90 B 93-90 D 95-83(1990) D 124-88 D 126 - 87(1991)" D 130 - 88 D 153-84(1989)" D 154-85(1989)" D 185-84(1989)" D 207-55(1987) D 209-81 (1989) D 210-81a(1991)" D 211-67(1989)" 212-87 D 215-9! D 233-65(1981)" D 234-82(1991)" D 235 - 87" Method of Salt Spray (Fog) Testing.............................. .................................................................. ...... 06.01 Method of Acetic Acid-Salt Spray (Fog) Testing (Discontinued 1988t--Replaced by Practice G 85) .. 06.01 Specification for Raw Tung Oil.................. ............................................................. ,.............................06.03 Specification for Spirits of Turpentine............ ..................................... ........................ .................... 06.03 Terminology Relating to Paint, Varnish, Lacquer, and Related Products ........................ 06.01, 06.02, 06.03 Test Methods for Sampling and Testing Lac Resins...................... .......'...................................................06.02 Practice for Chemical Analysis of White Pigments............................................................................ . 06.02 Test Methods of Chemical Analysis of Red Lead......................................................................................06.02 Test Methods of Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese............................. ............................................... ...............................................................06.02 Test Method for Flash Point by Tag Closed Tester...................................;............................................ 06.03 Specification for Zinc Oxide Pigments..................................................................................................... 06.02 Specification for Basic Carbonate White Lead Pigment........................................................................... 06.02 Specification for Red Lead Pigment ..........................................................................................................06.02 Specification for Ochre Pigment................................................................................................... ............. 06.02 Test Method for Distillation of Petroleum Products .......................... .................................... .......... 06.03 Test Methods for Flash Point by Pensky-Martens Closed Tester....................................................... . 06.93 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation..........06.01, 06.03' Specification for Degummed Soybean Oil.............................................. ............................. ..................... 06.03 Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium Oxide Green.......................................................... ............................................................... 06.02 Method for Detection of Copper Corrosion from Petroleum Products by the Copper Strip Tarnish Test................................... :.................................................................................................................... 06.03 Test Methods for Specific Gravity of Pigments.......................................... ..........................................06,02 Guide for Testing Varnishes...........................................................................................................06.01 Test Methods for Coarse Particles in Pigments, Pastes, and Paints............................................... 06.01, 06.02 Specification for Dry Bleached Lac.................... ........................................................... ........................06.02 Specification for Lampblack Pigment...................... ,....:..........................'......... ...: -- ................ 06.02 Specification fpr Bone Black Pigment............ ....................................................................................... .. . Jo-M Specification for Chrome Yellow and Chrome Grange Pigments ........................................ ................... 06.02 Specification for Chrome Green Pigment.................... ;;........... , : ...... 06.02 Methods of Chemical Analysis of White Linseed Oil Paint's.............................. ............................. ; Methods of Sampling and Testing Turpentine ................................................. 06.03 Specification for Raw Linseed Oil.................. .................... 06.03 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent}- ............... 06113 Approved for use by agencies ofthe Department of Defense and, ifindicated on the standard, replaces corresponding Federal or Military document Consult the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department of Defense. t Although this standard has been officially withdrawn from Society approval, a brief description is included for informa on on y. t-- D D D D D D D D D D D D D D D D P D D D D D E D D E E E E E E E C D E E r E r r ] i i i i i P i P t i i i i P r r i i i P I P DUP050297162 D 237-91 p 260 - 86 (1990) D 261-75(1987)" D 262 - 81 (1987)" D 263 - 75 (1987) D 267-82(1987)" D 268 - 90 D 269 - (1987)" D 279 - 87(1991)" D 280-81 (1987) D 281 - 84 (1989) D 283 - 84 (1990)" D 284-88 D 301 -89 D 302 - 85 D 303 - 85 D 304 - 90 D 305 - 84 (1990)" D 319-90 D 329 - 90 D 330 - 89 D 331 -90 D 332 - 87 (1991)" D 333 - 87 D 344 - 89 D 358-83(1988) D 360 - 89 D 362 - 84 D 363-90 D 365-84(1989)" D 387 - 86 D 411 -83(1987) D 444 - 88 D 464 - 91 D 465-82(1987)" D 475-67(1989) D 476 - 84 (1989) D 477-78 D 478 - 86 (1991)" D 480 - 88 D 509 - 70(1987) D 520-84(1989) D 521 - 90 D 522- 88" D 523 - 89 D 555-84(1988)" D 561 - 82 (1989) D 562 - 81 (1990)" D 563 - 88 D 564 - 87 (1991)" D 600-90 D 601 -87(1991)" D 602 - 81 (1991)" D 603-66(1989) D 604-81 (1989) D 605-82(1989) D 607 - 82 (1987)" D 608 - 90 D 609-90 D 610-85(1989)" D 611 -82(1987)2 D 656-87 D 658 - 91 D 659 - 86" D 660 - 87 CONTENTS, VOLUMES 06.07, 06.02, AND 06.03 Specification for Orange Shellac and Other Lacs.................................................................................. 06.02 Specification for Boiled Linseed Oil.......................................................................................................06.03 Specification for Iron Blue Pigment ...............................................................................................................06.02 Specification for Ultramarfine Blue Pigment.................................................................................................06.02 Specification for Chrome Oxide Green Pigment .......................................................................................... 06.02 Specification for Gold Bronze Powder...................................................................................................06.02 Methods of Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Materials ................................................................................................................06.03 Test Method for Toluene-Insoluble Solid Matter in Rosin (Chiefly Sand, Chips, Dirt, and Bark)... 06.03 Test Methods for Bleeding of Pigments .................................................................... Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments.......................................................................................................................... Test Method for Oil Adsorption of Pigments by Spatula Rub-Out ....................................................... 06.02 Test Methods for Chemical Analysis of Cuprous Oxide and CopperPigments.......................................... 06.02 Test Methods for Chemical Analysis of Mercuric Oxide Pigment ..............................................................06.02 Test Methods for Soluble Cellulose Nitrate ............................................................... Specification for Ethyl Acetate (85 to 88 % Grade) (DiscontinuedI987f--Replaced by Specification D4614)............................................................................................... Specification of n-Butyl Acetate (90 tb 92 % Grade) (Discontinued 1987f--Repaced by Specification D 4615)............................................. :.................................... ,................................................................ 06.03 Specification for n-Butyl Alcohol (Butanol) ................................................................... Test Method for Solvent-Extractable Material in Black Pigments ..............................................................06.02 Specification for Amyl Alcohol (Synthetic) '..................................................... 1........................................ 06.03 Specification for Acetone ............................................................................................ Specification for 2-Butoxyethanol...................................................................................................................06.03 Specification for 2-Ethoxyethanol ........................................................................................... Test Method for Relative Tinting Strength of White Pigments by VisualObservation...............................06.02 Test Methods for Clear and Pigmented Lacquers ................................................................ Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts....................... 06.01 Specification for Wood to Be Used as Panels in Weathering Tests of Coatings ....................................... 06.01 Specification for Shellac Varnishes................................................................... Specification for Industrial Grade Toluene (See Section on Aromatic Hydrocarbons) ............................. 06.03 Specification for Tricresyl Phosphate ............................................................ Methods of Testing Soluble Nitrocellulose Base Solutions .......................................................................... 06.02 Test Method for Color and Strength of Color Pigments with a Mechanical Muller ................................ 06.02. Methods of Testing Shellac Used for Electrical Insulation .......................................................................... 06.02 Test Methods for Chemical Analysis of Zinc Yellow Pigment (Zinc Chromate Yellow) ......................... 063)2 Test Methods for Saponification Number of Naval Store Products Including Tall Oil and Other Related Products ....................................................................................... :.................................................... ;.. 06.03 Test Methods for Acid Number of Rosin ..................................................................... Specification for Pure Para Red Toner Pigments ........................................................................................ 06.02 Specification for Titanium Dioxide Pigments ...................................................................... Specification for Zinc Sulfide Pigmentrs (Discontinued 1988f) ..................................................................06.02 Specification for Zinc Yellow (Zinc Chromate) Pigments..................................................... Test Methods for Sampling and Testing of Flaked Aluminum Powders and Pastes ............................. 06.03 Test Methods of Sampling and Grading Rosin .................................................. Specification for Zinc Dust Pigment ..............r........................................................................................... 06.02 Methods for Chemical Analysis of Zinc Dust (metallic Zinc Powder) . ....................................................06.02 Test Methods for Mandrel Bend Test of Attached Organic Coatings..........................................................06.01 Test Method for Specular Gloss ....................................................................................... Guide for Testing Drying Oils ..... -- i.............................................................. Specification for Carbon Black Pigment for Paint............. Test Method for Consistency of Paints Using the Stormer Viscometef .....................................'.............06.01 Test Method for Phthalic Anhydride Content of Alkyd Resins and Resin Solutions ............................. 06.02 Test Method for Liquid Paint Driers ........ I'Y.......... ............................................. .................................... 06.03 Specification for Liquid Paint Driers ..................................................................... Specification for Oiticica Oil (Permanently Liquid) ...................... .................. .:................ ............ 06.03 Specification for Barium Sulfate Pigments ......................................................................................... 06.02- Specification for Aluminum Silicate Pigments- (Hydrous)......................................................... Specification for Diatomaceous Silica Pigment ..................................................... Specification for Magnesium Silicate Pigment (Talc) .................................................................................. 06.02 Specification for Wet Ground Mica Pigments . t.....-........................................................ Specification for Dibutyl Phthalate................. ........ .....................................'................................... 06.03 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer and Related Products .. 06.01 Test Methods for Evaluating Degree of Rusting on Painted Steel Surfaces ............................................... 06.01 Test Methods for Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents ............................................................... L ........... ....................................................... . 06.03 Specification for Pure Toluidine Red Toner ............ .................................. ........................................ ... 063)2 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive ................................... 06.01 Method of Evaluating Degree of Chalking of Exterior Paints (Discontinued 1990t--Replaced by Test Methods D4214) ... ...-.................... .................. ..............................................................\ . 06.01 Test Method for Evaluating Degree of Checking of Exterior Paints............................................................06.01 xi 06 06.02 06 06.03 06. 06.03 06.01 06.03 06.02 06.02 . 06.0 06.01 06 06.02 06.02 0 06.02 DUP050297163 t 661 - 86el SD 662 - 86" D 711- 89 D 713 - 90 D 714- 87 D 715- 86(1991)" 86(1991)" 86(1991)" 86(1991)" 91 89 81 (1988)" 87(1991)" D 768 81(1987)" D 769 87(1991)" D 770 90 D 772 86" D 784 83(1987) D 801 57(1987) D 802 82(1987) D 803 82(1987) D 804 79(1987) D 817 91 D 822 89 D 823-91 49(1987) 81(1986)" 85(1989)" 85(1989)" 87 91 58 (1987) 58(1987) 87 81 (1986) , gg 72(1989)" 79(1988) 86 81(1986)" 81 (1986)" 65(1989) -81 (1991 )*2 -85(1989)" -86(1991)" D 1005 -84(1990)" D 1006 73(1986)" D1007 -90 D l013 - 88 D 1014 - 83(1988)" D 1063 51 (1987) D 1064- -58(1981) D 1065 -82 D 1078 -86 D 1131 -53(1981)" D 1133 -90 D 1135 -86(1991)" D1150 -55(1987)" D 1152 -89 01153 -90 01155 -89 D 1186 -87 D 1193-91 D1198 - 88 D1199 - 86 (1991)" D 1200 - 88 D 1208 - 84 (1989)" D 1209 - 84 (1988)" CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Test Method for Evaluating Degree of Cracking of Exterior Paints___ n Test Method for Evaluating Degree of Erosion of Exterior Paints.......................................................... Test Method for No-Pick-Up Time of Traffic Paint..............................!!!!!!.]................................... "*"* Practice for Conducting Road Service Tests on Fluid Traffic Marking Materials....................................n* 2J Test Method for Evaluating Degree of Blistering of Paints.................. ..................................J Test Methods for Analysis of Barium Sulfate Pigment........................\\................................................. ..... Test Methods for Evaluating Mica Pigment.................................... \\\\.................................................JJJHlf Test Methods for Analysis of Magnesium Silicate Pigment................ ............................................... JJrJJf Test Methods for Analysis of Aluminum Silicate Pigment...................... ' ........................................ Test Methods for Analysis of Diatomaceous Silica Pigment................................................................... 06 02 Specification for Methyl Ethyl Ketone...................................................... .................................. 06 03 Specification for Raw and Burnt Umber Pigments ................................] ... ...........................................q A, Specification for Raw and Burnt Sienna Pigments..........................................' "................................. w Specification for Yellow Iron Oxide Hydrated.............................................. ......................................0^02 Specification for Black Synthetic Iron Oxide........................................................................................... wj)2 Specification for Isopropyl Alcohol.......... ............................................................. ................................' 06J)3 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints............ . Specification for Orange Shellac and Other Indian Lacs for Electrical Insulation 06.01 .................... 06.02 Test Methods for Sampling and Testing Dipentene..............................................!!!.!!....................... 06.03 Test Methods for Sampling and Testing Pine Oil.................................................... 063)3 Test Methods for Testing Tall Oil............................................ ....................................063)3 Definitions of Terms Relating to Naval Stores and Related Pfoducts................................. 063)3 Methods ofTesting Cellulose Acetate Propionate and Cellulose Acetate Butyrate063)2 Practice for Conducting Tests on Paint and Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light and Water Exposure Apparatus............................................................................... 06.01 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels ............................................................................... ...............................................................06.01 Test Methods for Sampling and Testing Pine Tars and Pine-Tar Oils (Intent to Withdraw).................. 06.03 Specification for Pumice Pigment................................................................................................................ 06.02 Test Method for Evaluating Degree of Bleeding of Traffic Paint............................................................... 06.01 Test Method for Evaluating Degree of Settling of Paint............................................................................. 06.01 Practice for Testing Water Resistance of Coatings Using Water Immersion............................................ 063)1 Methods of Testing Cellulose Acetate.................................... ...................................................................06.02 Test Method for Volatile Oil in Rosin ......................................................................................................06.03 Test Method for Water in Liquid Naval Stores........................................................................................ 063)3 Specification for Mercuric Oxide for Use in Antifouling Paints................................................................06.02 Specification for Cuprous Oxide for Use in Antifouling Paints................................................................. 063)2 Test Method for Evaluating Degree of Resistance to Wear of Traffic Paint............................................. 063)1 Test Methods for Ethylcellulose................................................................................................................... 063)2 Specification for Raw Castor Oil................................................................................................................ 06.03 Specification for Dehydrated Castor Oil.............. ..................................................................................... 063)3 Specification for Aluminum Powder and Paste Pigments for Paints........................................................ 06.02 Specification for Copper Phthalocyanine Blue Pigment............................................................................. 063)2 Specification for Copper Powder for Use in Antifouling Paints................................................................ 063)2 Test Methods for Abrasion Resistance ofOrganic Coatings by Falling Abrasive.................................... 063)1 . Test Method for Laboratory Determination of Degree of Bleeding of Traffic Paint .............................. 063)1 Test Methods for Para Red and Toluidine Red Pigments........................................................................ 06.02 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers........ 06.01 Practice for Conducting Exterior Exposure Tests of Paints on Wood ................ ................................ 063)1 Specification for sec-Butyl Alcohol...................................... ...................................................................... Test Method for Determining Total Nitrogen in Resins and Plastics...................................................... 06.02 Test Method for Conducting Exterior Exposure Tests of Paints on Steel................................................ 06.01 Test Method for Ash in Rosin....................................... ........................................................................ Test Method for Iron in Rosin................ .......... .................................... .............................................. Test Methods for Unsaponifiable Matter in Rosm............ ........................ ............................................ 06.2> Test Method for Distillation Range of Volatile Organic Liquids............................ ..................................63 Methods of Testing Rosin Oils..................................................................................................................... Test Method for Kauri-Butanol Value of Hydrocarbon Solvents............................................................ 06-3 Test Methods for Chemical Analysis of Blue Pigments ................ ............................................................ Single- and Multi-Panel Forms for Recording Results of Exposure Tests ofPaints................................ 063)1 Specification for Methanol (Methyl Alcohol).............................................................................................Vy""f Specification for Methyl Isobutyl Ketone........ .......................................................................................... Otow Test Method for Roundness of Glass Spheres.................................................. ..............W*U2 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base .............................. ............. ........................................................................ - Specification for Reagent Water............ ............ ...................................................................................... Test Method for Solvent Tolerance of Amine Resins.................. .............................................................. Specification for Calcium Carbonate Pigments............................ .............................................................. 06.02 Test Method for Viscosity by Ford Viscosity Cup.............. ................................................................... 6-lU Test Methods for Common Properties of Certain Pigments........................................................... <.02 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)................................................. 06.01,06.03 xu. DUP050297164 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 r D 1210-79(1988)*' D 1211 -87 Test Method for Fineness of Dispersion of Pigment-Vehicle Systems................................................... 06.01 Test Method for Temperature-Change Resistance of Clear NitrocelluloseLacquer FilmsApplied to Wood.............................................................................................................................................................06.01 D 1212 - 91 Methods for Measurement of Wet Film Thickness of Organic Coatings.......................................................06.01 D 1214 - 89 Test Method for Sieve Analysis of Glass Spheres...........................................................................................06.02 D 1240-82 Test Method for Rosin Acids in Fatty Adds ................................................................................................. 06.03 D 1257 - 90 Specification for High-Gravity Glycerin......................................................................................................... 06.03 D 1258 - 90 D 1259 - 85 (1990)*' Test Methods for Testing High-Gravity Glycerin...........................................................................................06.03 Test Methods for Nonvolatile Content of Resin Solutions ...........................................................................064)2 r D 1296 - 84 (1988)*' Test Method for Odor of Volatile Solvents and Diluents...............................................................................06.03 D 1301 - 91 Test Methods for Chemical Analysis of White Lead Pigments.................................................................... 06.02 D 1306 - 88 Test Method for Phthalic Anhydride Content of Alkyd Resins and EstersContaining Other Dibasic Adds (Gravimetric)...................................................................................................................................... 06.02 D 1308 - 87 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes ................... 06.01 D1309 - 88 Test Method for Settling Properties of Traffic Paints During Storage................................................... 06.01 D 1310 - 86 (1990)*' Test Method for Flash Point and Fixe Points of Liquids by Tag Open-Cup Apparatus..............................06.03 D1312 - 56 (1987)*' Test Methods for Apparent Free Phenols in Synthetic Phenolic Resins or Solutions Used for Coating Purposes.........................................................................................................................................................06.02 D 1316 - 87 Test Method for fineness of Grind of Printing Inks by the NPIRI Grindometer..................................... 06.01 D 1343 - 91 D1347 - 72 (1989)*' Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method..................................................06.02 Test Methods for Methylcellulose............................................................................................................06.02 V D1348 - 89 Test Methods for Moisture in Cellulose.................. '.................................................................................. 06.02 D 1353 - 90 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Related Products................................................... 06>03 D1358 - 86 Test Method for Spectrophotometric Diene Value of Dehydrated Castor Oil and Its Derivatives..........06.03 D1360 - 90a Test Method for Fire Retardancy of Paints (Cabinet Method) ............................................................ 06.01 D 1363 - 88 Test Method for Permanganate Time ofAcetone and Methanol ................................................................06.03 D 1364 - 90 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)..................................... 06.03 D 1366 - 86 (1991)61 Practice for Reporting Particle Size Characteristics of Pigments................. 06.02 D 1392 - 87 Specification for Safflower Oil......................................................................................................................... 06.03 D1394-76(1991)*` Test Methods for Chemical Analysis of White Titanium Pigments.......................................................06.02 D1395 - 58 (1974) Test Method for Abrasion Resistance of Clear Floor Coatings(Discontinued 1989t).................................06.01 D1396 - 73 (1987)*' Test Methods for Chemical Analysis of Poly(Vinyl Butyral).........................................................................06.02 D 1397 - 88 Test Method for Unsaponifiable Matter in Alkyd Resinsand ResinSolutions ........................................... 06.02 D 1398 - 84 Test Method for Fatty Add Content of Alkyd Resins and AlkydResinSolutions ..................................... 06.02 6 t D1399 - 90 D 1400 - 87 Test Method for Unsaponifiable Content of Tricresyl Phosphate....... ........................................................ 06.03 Test Method for Nondestructive Measurement of Dry film Thickness ofNonconductive Coatings < D1439 - 83a (1989)*' Applied to a Nonferrous Metal Base.......................................................................................................... 06.01 Test Methods for Sodium Carboxymethylcellulose......................................................................................... 06.02 5 D1462 - 87 Specification for Refined Soybean Oil............................................................................................................. 06.03 j D1466 - 86 Test Method for Sampling Liquid Oils and Fatty AddsCommonly Used in Paints,Varnishes, and i Related Materials........................................................................................................................................ 06.03 2 D1467 - 89 . Guide for Testing Fatty Adds Used in Protective Coatings......................................................................... 06.03 2 D 1468 - 84 (1988)*' Test Method for Volatile Matter in Tricresyl Phosphate ...............................................................................06.03 1 D1469 - 73 (1988)*' Test Method for Total Rosin Acids Content of Coating Vehicles................................................................ 06.02 1 D 1474 - 85 (1991)*' Test Methods for Indentation Hardness ofOrganic Coatings.......................................................................06.01 2 D 1475 - 90 Test Method for Density of Paint, Varnish, Lacquer, and Related Products.............................................. 06.01 1 D 1476 - 88 Test Method for Heptane Misdbility of Lacquer Solvents.............................................................................06.03 1 D1483 - 84 (1989)*' Test Method for Oil Absorption of Figments by Gardner-Coleraan Method..............................................06.02 3 D 1537 - 60 (1988)*' Specification for Distilled Soybean Fatty Acids............................................................................................ 06.03 2 D1538 - 60 (1988)*' Specification for Distilled Linseed Fatty Adds .....:....................................................................................06.03 1 D 1539 - 60 (1988) Spedfication for Dehydrated Castor Acids.............................................................................................. 06.03 3 D 1540 - 82 (1987)*' Practice for Effect of Chemical Agents on Organic Finishes Used.inthe Transportation Industry......... 06.01 3 D 1541 - 86 Test Method for Total Iodine Value of Drying Oils and Their Derivatives................................................06.03 3 D 1542 - 60 (1988)*' Test Method for Qualitative Detection of Rosin in Varnishes.......................................................... 06.01,06.02 3 D 1543 - 86 Test Method for Color Permanence of White Architectural Enamels (Discontinued 1992f) ................... 06.01 3 >3 D 1545 - 89 Test Method for Viscosity of Transparent Liquids by Bubble Time Method..................... 06.01,06.02, 06.03 12 D 1546 - 62 (1987) Method for Performance Tests of Clear Floor Sealers ..................................................................................06.01 1 D 1585 - 82 Test Methods for Fatty Adds Content ofTall Oil Rosin............................................................................ 064)3 )3 D 1612 - 90 Test Method for Acetone in Methanol (Methyl Alcohol)........................ 064)3 13 D 1613-91 Test Method for Aridity in Volatile Solvents and'Chemical Intermediates Used in Paint, Varnish, 22 Lacquer, and Related Products .................................................................................................. ..............06.03 D1614-9I Test Method for Alkalinity in Acetone......................................................................................... 064)3 31 D1615 - 60 (1987) Test Methods for Glycerol, Ethylene Glycol, and Pentaerythritol in Alkyd Resins....................................06.02 33 D 1617 - 90 Test Method for Ester Value of Solvents and Thinners ................................................................................ 06.03 32 D 1638 - 74*' Methods of Testing Urethane Foam Isocyanate Raw Materials (Discontinued 199 If)..............................06.03 02 D 1639 - 90 ' Test Method for Acid Value of Organic Coating Materials ............................................. ........................06-01 01 D 1640 - 83 (1989)*' Test Methods for Drying, Curing or Film Formation of Organic Coatings at Room Temperature .... 06.01 02 D 1641 - 59(1987) Test Method for Exterior Durability ofVarnishes.......... ....................................................... ...............06.01 03 D 1642 - 70 (1987) Test Methods for Elasticity or Toughness of Varnishes ...................................................... 1....................06.01 k xm DUPQ50297165 D 1643-60(1988) D 1644 - 88 D 1647 - 89 D1648 - 86 D 1649 - 82(1987)" D 1650 - 91 D 1652 - 90 D 1653-91a D 1654- 79a (1984)" D 1695 - 77 (1989)" D 1696-90 D 1716-62(1987) D 1718-86 D 1719-90 D 1720-88 01721 -84(1988)" 01722-90 0 1725 - 62(1989)" 01726-90 D 1728 - 83 D 1730 - 67(1984)" D 1731-67 (1984)" D 1732-67(1984) D 1734-63(1980)" D 1735-87 D 1736-89 D 1737-85 0 1787 - 89 01794-89 D 1795-90 01836-91 0 1841-63(1988)" 0 1842 - 63(1988) D 1843 - 63(1988)" D 1844-86(1991)" D 1845-86 (1991)" D 1847 - 87 D 1848 - 88 D 1849-80(1987)" D 1915-63(1989)" D 1926-89 D 1950-86 D 1951-86 D 1952-86 D 1954-86 D 1955 - 85(1989)" D1957 - 86 D 1958 - 86 (1990) D 1959-85(1989)" D 1960-86(1990) D 1962 - 85 (1989)" D 1963 - 85(1989)" D 1964-85 (1989)" D 1965 -87 (1991)" D 1966-69(1991)" D 1967 -86 D 1969 - 91 D 1978-91 D 1979 - 91 D 1980 - 87(1991)" D 1981 - 86 (1990) D 1982-85 (1989)" D 1983-90 D 1984-69(1988) D 2064-91 D 2065-91 02066-91 D 2071 -87(1991)" CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Test Methods for Gas Checking and Draft Test of Varnish Film* Test Methods for Nonvolatile Content of Varnishes ......................................................... 06.01 Test Methods for Resistance of Dried Films of Varnishes to Water and Altai!..................................... 9&l Specification for Basic Lead Silicochromate Pigment AUcalt ....................................06.01 Specification for Strontium Chromate Pigment........ | ........................................................................... ... Methods of Sampling and Testing Shellac Varnish .................................................................................064)2 Test Method for Epoxy Content of Epoxy Resins ................................................................................ Test Methods for Water Vapor Transmission of Otganic Coating Fiinw................................................. 6.02 Method for Evaluation of Painted or Coated Specimens Subjected '.............................061)1 Terminology of Cellulose and Cellulose DerivativTM Jected t0 CoiTOS,ve Envuoninems .......... Test Method for Solubility of Cellulose in Sodium Hydroxide............................................................... Test Method for Cellulose Chain Length Uniformity by Fractional W V `' ^rLL'' * Sr?? Specification for Isobutyl Acetate (95 % Grade) . * Dal PreClpitatlon of C*TM0* Nitrate . 06.02 Specification for Isobutyl Alcohol.................................... ........................................................... "6-03 Test Method for Dilution Ratio of Active Solvents in CeUulose Nitrate Srfutinnt................................. Test Method for Permanganate Time ofTricresyl Phosphate ............................... Test Method for Water Miscibility of Water-Soluble Solvents ...............................................................K Test Method for Viscosity of Resin Solutions (Intent to Withdraw))..................................................... iwlS Test Method for Hydrolyzable Chlorine Content of Liquid Eooxv Reins.............................................Sm Test Method for Phthalate Ester Color ofHigh-Gravity Glycerin (Discontinued 1991+)..........................EXJ Practices for Preparation of Aluminum and Aluminum Surfaces for Paintum IS nt Practices for Preparation of Hot-Dip Aluminum Surfhces for Painting .. ..................................... ngn! Practices for Preparation of Magnesium Alloy Surfaces for Painting ..................................................... Method of Making and Preparing Concrete and Masonry Panels for Testina PaintFinkh^................nUnt Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus .... ................S39 Test Method for Efflorescence of Interior Wall Paints ..................................... .................................... 06.01 Test Method for Elongation of Attached Organic Coatings with CylindricalMandrel Aooaratus (Discontinued 1988t--Replaced by Test Methods D 522) ....................................... 06J)t Test Method for Pentosans in Cellulose....................................................... .......................................... 06JB Test Method for Alcohol-Benzene Soluble Matter in Cellulose (Intent to Whhdrawt) Test Method for Intrinsic Viscosity of Cellulose .......................................................................... '' osjft Specification for Commercial Hexanes ................................................................................ "........... ] 06A3 Specification for Distilled Coconut Fatty Acids.................................................................. 064)3 Specification for Distilled Corn Fatty Acids............................................... ...........................06.03 Specification for Fractionated and Distilled Cottonseed Fatty Acids .................................................... 06A3 Test Methods for Chemical Analysis of Basic Lead Silicochromate........................................................064)2 Test Methods for Chemical Analysis of Strontium Chromate Pigment .................................................. 064)2 Test Method for Total Chlorine Content of Epoxy Resins....................................................................064)2 Classification for Reporting Paint Film Failures Characteristic of Exterior Latex Paints ..................... 064)1 Test Method for Package Stability of Paint ............................................................................................06411 Method for Chromatographic Analysis of Chemically Refined CeUulose ............................................ 06412 Test Methods for Carboxyl Content of CeUulose .................................................................................. 064)2 Test Method for Acetone Tolerance of Heat-Bodied Drying Oils ........................................................ 064)3 Test Method for Ash in Drying Oils and Fatty Adds .......... 064)3 Test Method for Quantitative Determination of Break in Drying Oils ............ .................................... 064B Test Method for Foots in Raw Linseed OU (Volumetric Method)........................................................ 66413 Test Method for Gel Time of Drying Oils .............................................................................................. 664Q Test Method for Hydroxyl Value of Fatty Oils and Adds ...:.......... ..................................................06a3 Test Method for Chloroform Insoluble Matter in Oitidca Oil .............................................................. 064J3 Test Method for Iodine Value of Drying Oils and Fatty Adds : --................................................... 064w Test Method for Loss on Heating of Drying Oils.......................... ;"........J"* Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty tods .... 6640 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/ 25C ................ * ........... ...................................... O9 4 Test Method Ibr U^apod^We'Matter in Drying Oik, Fatty Adds, and Polymerized Fatty to* .. - 064)3 Test Method for Foots in Raw Linseed OU (Gravimetric Method) .......................................................* Test Method for Measuring Color After Heating of Drying Oils .......................................................... S9 Specification for 2-Ethylhetanol (Synthetic) ............................................................................................... Guide for Analysis of Electrocoat Bath Samples ................................................................ 9 9 Test Method for Free Formaldehyde Content of Amino Resms ............................................... ncjn. Test Method for Acid Value of Fatty Acids and Polgnerized Fatty Aads ........................................... < Test Method for Measuring Color After Heating of Fatty Adds .............................................. 06.63 Trat Method for Fatty Add Composition by Gas-Liquid Chromatograph of Methyl Esters * ^ Specification for Tall Oil Fatty Acids .. ............................................... ............... QtMi 55 B5B g gsaar/tfS5SL MiiiS 4 TMtNMw*MMMiwrlillNfliwiii*4Antingilkttiinw ..........till. Test Methods for Fatty Nitrogen Products ................ -......................... ......................... D2 D2 D2 SD2< D2` D2 D2 D2 D2 D2 D2 D2 D2 D21 D2I D21 D22 D22 D22 D22 D22 SD22 D22 D22 D22 D 22 D 23 D2t D2. D2: D23 D23 D23 D23 D23 . " D23i D23f D23f D23f SD236 D237 D237 1 D237 D237 . D237 *>237 D237 D237 ' D237 D238< i D243 ` DUP050297166 6.01 6.01 6.01 6.02 6.02 6.02 6.02 6.01 6.01 6.02 6.02 6.02 6.03 6.03 6.03 6.03 6.03 6.02 6.02 6.03 6.01 $.01 $.01 $.01 $.01 $.01 SDl $.02 5J)2 $.02 $.03 5.03 $.03 $.03 $.02 $.02 $.02 $.01 $.01 $.02 $J>2 $.03 >D3 $.03 03 03 03 03 03 03 03 ..03 $.03 1.03 $.03 $.03 $.03 $.01 $.02 $.03 ..03 1.03 $.03 >.03 $.01 01 >.01 >.03 D 2072 - 66 (1987)1 D 2073-66 (1987)1 D 2074 - 66 (1987)e 1 ^ D 2075 - 89 D 2076 - 64 (I987)e` D 2077 - 64 (1987) D 2078 - 86 (1990) D 2079 - 82 (1987) D 2080 - 64 (1987) D 2081 - 64 (1987) D 2082 - 82 (1987) 0 2083 - 66(1987) D 2086 - 89 D 2087 - 89 D 2090 - 88 D2091 - 88 D 2092 - 86 D 2134 - 66 (1980)ei D 2190 - 89 D2191-89 D 2192 - 89 D 2193 - 89 D 2194 - 89 D2195-89 1 D 2196 -86(1991)" D2197 - 86 (1991)l ! D2198-84(1989)1 j D 2199 - 82 (1987) ; D 2200 - 91 j D 2201 - 65 (1987)l j | D 2205 - 85 (1990)1 D2218 - 67(1989)1 | D 2243 - 90 D 2244 - 89 ! D 2245 - 90 j D 2246 - 87 j D 2247 - 87 D 2248 - 89 D 2336 - 87 (1991)el D 2337 - 84 (1989) D2338 - 84 (I989)l D 2348 - 91 D 2349 - 90 ' D2350 - 90 I D 2351 - 90 'D 2352 - 85 (1990)1 D 2353 - 83 D 2354 - 91 D 2363 - 79 (1989)l D 2364 - 89 D 2366 -68 (1980)l D 2369 - 90 D2370 - 82 (1987)a D2371 - 85 (1990)I D2372 - 85 (1990)1 D 2373 - 85 (1990)61 D 2374 - 85 (1990)l D 2375 - 85 (1990)1 D2376 - 84 (1989) D2378 - 84 (1987) D2379 - 84 (1987) D 2380 - 84 (1987) D 2438 - 89 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Test Method for Water in Fatty Nitrogen Compounds................................................................................ 06.03 Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines, Amidoamines, and Diamines by Referee Potentiometric Method.........................................................06.03 Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines by Alternative Indicator Method........................................................................................ .............................................. 06.03 Test Method for Iodine Value of Fatty Amines, Amidoamines, and Diamines......................................... 06.03 Test Methods for Acid Value and Amine Value of Fatty Quaternary Ammonium Chlorides ................. 06.03 Test Method for Ash in Fatty Quaternary Ammonium Chlorides ........................................................... 06.03 Test Method for Iodine Value of Fatty Quaternary Ammonium Chlorides............................................... 06.03 Test Method for Nonvolatile Matter (Solids) in Fatty Quaternary Ammonium Chlorides....................... 06.03 Test Method for Average Molecular Weight of Fatty Quaternary Ammonium Chlorides......................... 06.03 Test Method for pH of Fatty Quaternary Ammonium Chlorides................................................................06.03 Test Method for Percent of Non-Amines in Fatty Nitrogen Compounds................................................... 06.03 Test Method for Calculation of Percent of Primary, Secondary, and Tertiary Amines in Fatty Amines.........................................................................................................................................................06.03 Test Method for Acidity in Vinyl Acetate and Acetaldehyde ...................................................................... 06.03 Test Method for Iron in Formaldehyde Solutions........................................................................................ 06.03 Test Method for Clarity and Cleanness of Paint and Ink Liquids....................................................06.02,06.03 Test Method for Print Resistance of Lacquers......................... .................................................................. 06.01 Practice for Preparation of Zinc-Coated (Galvanized) SteelSurfaces for Painting .................................... 06.01 Test Method for Softening of Organic Coatings by Plastic Compositions (Discontinued1990f)...............06.01 Specification for Vinyl Acetate ............................................. 06.03 Test Method for Acetaldehyde Content of Vinyl Acetate ............................................................................ 06.03 Test Method for Purity of Aldehydes and Ketones ..................... 06.03 Test Method for Hydroquinone in Vinyl Acetate.......................................................................................... 06.03 Test Method for Concentration of Formaldehyde Solutions........................................................................ 06.03 Test Methods for Pentaerythritol.................................................................................................................. 06.03 Test Methods for Rheological Properties of Non-NewtonianMaterials byRotational (Brookfield) Viscometer.................................................................................................................................................. 06.01 Test Method for Adhesion of Organic Coatings by Scrape Adhesion..........................................................06.01 Test Method for Stain Removal from Multicolor Lacquers............................... ........................................ 06.01 Method for Measurement of Plasticizer Migration from Vinyl Fabrics to Lacquers................................. 06.01 Pictorial Surface Preparation Standards for Painting Steel Surfaces........................................ 06.01 Test Method for Preparation of Hot-Dipped Nonpassivated GalvanizedSteel Panels for Testing Paint, Varnish, Lacquer, and Related Products...................................... ......................................................... 06.01 Guide for Selection of Tests for Traffic Paints....................... 06.01 Specification for Molybdate Orange Pigments...............................................................................................06.02 Test Method for Freeze-Thaw Resistance of Water-Borne Coatings............................................................06.01 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates.. 06.01 Test Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints................................... 06.03 Test Method for Finishes on Primed Metallic Substrates for Humidity-Thermal CycleCracking............ 06.01 Practice for Testing Water Resistance of Coatings in 100 % RelativeHumidity.........................................06.01 Practice for Detergent Resistance of Organic Finishes...................................................................................06.01 Practice for Specifying Properties from Liquid Through Cured State for Coatings Factory Applied to Wood Products............................................................................................................................................ 06.01 Test Method for Freeze-Thaw Stability of Multicolor Lacquers..................................................................06.01 Test Method for Determining Particle Size of Multicolor Lacquers............................................................06.01 Test Method for Arsenic in Paint............................... 06-01 Test Method of Qualitative Determination of Nature of Thinner in Solvent-Reducible Paints............. 06.01 Test Method for Antimony Oxide in White Pigment Separated from Solvent-Reducible Paints.............06.02 Test Method for Sulfide in White Pigment Separated from Solvent-Reducible Paints............................... 06.02 Test Method for Sulfur Dioxide in White Pigment Separated from Solvent-Reducible Paints................. 06.02 Test Method for Flow Ratings of Organic Coatings Using the Shell Flow Comparator (Discontinued 1992t)................................................... ........................................... .........................................................06.01 Test Method for Minimum Rim Formation Temperature (MFT) of Emulsion Vehicles......................... 06.02 Test Methods for Hydroxypropyl Methycellulose.......................................................................................... 06.02 Test Methods for Hydroxyethylcellulose...................... 06.02 Test Method for Accelerated Testing of Moisture Blister Resistance of Exterior House Paints on Wood (Discontinued 1989f) .............................................. 06.01 Test Method for Volatile Content of Coatings------'....:................. 06.01 Test Method for Tensile Properties of Organic Coatings....................... 06.01 Test Method for Pigment Content of Solvent-Reducible Paints......................................................... . 06.01 Practice of Separation of Vehicle from Solvent-Reducible Paints................................................................ 06.01 Test Method for Determination of Cobalt in Paint Driers by EDTA Method .......................................... 06.03 Test Method for Lead in Paint Driers by EDTA Method................. 06.03 Test Method for Manganese in Paint Driers by EDTA Method.................................................................. 06.03 Test Method for Slump of Face Glazing and Bedding Compounds on Metal Sash................................... <36.01 Specification for Formaldehyde 50 % Grade Uninhibited and 37 % Grade Inhibited and Uninhibited . 06.03 Test Method for Acidity of Formaldehyde Solutions......................................................................... 06.03 Test Method for Methanol Content of Formaldehyde Solutions.................................................................. 06.03 Test Method for Silica in Cellulose................................................................................................................. 06.02 XY DUP050297167 0 2448 - 85(1989) 0 2454 - 91 D 2455-89 D 2456-91 D 2485-91 D 2486-89 D 2571 -88 0 2572-91 0 2574-86 0 2575 - 70(1991)" 0 2613 - 85(1990)" 0 2620 - 87 D 2621-87 D 2627 - 91 D 2634 - 86 D 2635 - 91 D 2636-91 D 2641 - 89 D 2689 - 88 0 2690-89 D 2691 -88 D 2693 - 87 D 2694-87 D 2695 - 87 D 2696-87 D 2697 - 86 D 2698 - 90 D 2742 - 79 D 2743 - 68 (1987) D 2744 - 68 (1989)" D 2745 - 89 D 2792 - 69 (1987) D 2793-69 (1987) D 2794 - 90 D 2800-87 D 2801-69 (1981)" 0 2803 - 82(1987) 02804-88 02805-88 0 2830 - 91 0 2832 - 83(1991)" D 2833-89 D 2916-88 D 2917-91 02921 - 88 D 2929 - 89 0 2931-84(1989)" D 2932-80 (1988)" D 2933-74 (1986)" D 2998 89 02999 85 D 3002-81 (1987) D 3003 - 71 (1987) D 3008-90 D 3009 - 72 (1981)" D3021 - 82 (1987)" D 3022 - 84 (1989)" D 3023 - 88 D 3125-83 (1987) D 3126-83 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate Os^j of the Pigment.......................... ................................................................................................................. Practice for Determining the Effect of Overbaking on Organic Coatings.................................................O6.01 Test Method for Identification of Carboxylic Acids in Alkyd Resins.......................................................Qjgl Test Method for Identification of Polyhydric Alcohols in Alkyd Resins ................................................ Test Methods for Evaluating Coatings for High Temperature Service .................................................... o Test Method for Scrub Resistance of Interior Latex Flat Wall Paints .................................................... o $_5> Guide for Testing Wood Furniture Lacquers oeni Test Method for Isocyanate Groups in Urethane Materials or Prepolymers ............................... Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms Test Methods for Polymerized Fatty Acids ...... ............................................................................. Test Method for Calcium or Zinc in Paint Driers by EDTA Method ......................................... 06.92 Ml 064)3 06H3 Test Method for Light Stability of Clear Coatings......................................................................... Test Method for Infrared Identification of Vehicle Solids from Solvent-Reducible Paints........ 06411 0681 Specification for Diacetone Alcohol ............................................................................................... 0683 Specification Specification Specification for for for Methyl Amyl Acetate (95 % Grade)'.................................................................... Methyl Isobutyl Carbinol .................... .............................................................. Hexylene Glycol ............................................................................................................ 06.03 jjj0y6j.i0j3 Test Method for Chlorine in Cellulose...................................................................................................... Practices for Testing Alkyd Resins .............................................................................................................6> 7> Test Method for Isophthalic Acid in Alkyd and Polyester Resins .......................................................... Test Methods for Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products . 068] Specification for Ethylene Glycol .............................................................................................................. 0683 Specification for Diethylene Glycol ............ ............................................................................................. 0683 Specification for Propylene Glycol (Discontinued 1992+)......................................................................... 06.03 Specification for Dipropylene Glycol (Discontinued1992+).......................................................................06jll3 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings..................................... 0681 Method for Determination of the Pigment" Content of Solvent-Reducible Paints by High-Speed Centrifuging .............................................................................................................................................06.01 Methods for Chemical Analysis of Tribasic Lead Phosphosilicate (Discontinued 1990+)..................... 66J& Practices for Uniformity of Traffic Paint Vehicle Solids by Spectroscopy and Gas Chromatography .. 6681 Specification for Tribasic Lead Phosphosilicate (Discontinued 1988+) ............................................. (1682 Test Method for Relative Tinting Strength of White Pigments by Reflectance Measurements...............0682 Test Method for Solvent and Fuel Resistance of Traffic Paint................................................................. 0681 Test Method for Block Resistance of Organic Coatings on Wood Substrates ....................................... 0681 Test Method for Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact)..........068! Test Method for Preparation of Methyl Esters from Oils for Determination of Fatty Acid Composition V. by Gas Chromatography........ ............................................................................................................... 0683k Test Method for Leveling Characteristics of Paints:by Draw-Down Method (Discontinued 1990+) ... 068! Test Method for Filiform Corrosion Resistance of Organic Coatings on Metal ...................................0681'- Test Method for Purity of Methyl Ethyl Ketone by Gas Chromatography ............................................ 0683 Test Method for Hiding Power of Paints by Reflectometry .................................................................... 0681 ' Test Method for Durability and Compatibility of Factory-Primed Wood Products with Representative ' Finish Coats ........ 0681 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings ................... 06.01 Index of Methods for Testing Architectural Paints and Coatings........................................................... 06.01 Specification for Isophorone .......................................... 0683 Specification for Methyl Isoamyl Ketone............................................................................ _................... 0601 Test Method for Qualitative Tests for the Presence of Water Repellents and Preservatives in Wood Products ................ ..............................................................................................:..................................0681a Test Method for Sulfur Content of Cellulosic Materials by X-ray Fluorescence .'................................. 0682 Guide for Testing Latex Flat Wall Paints . .................................... _.................................................... 0681 Guide for Testing Exterior Solvent-Reducible House and Trim Coatings ................-- ...................0681 Test Method for Corrosion Resistance ofCoated Steel Specimens (Cyclic Method) (Discontinued 1992+) ................................................................... ..0681 Test Method for Polyhydric Alcohols in Alkyd Resins................ ---------------- :............................. 0683 Test Method for Monopentaerythritol in Commercial Pentaerythritol (Discontinued 1989+--Replaced by Test Method D 2195).......................................... ............................................................ ............... 0683 Practice for Evaluation of Coatings for Plastics -- ......................... _......... _........... ............. 0681 Test Method for Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates . 06814 Test Method for Resin Adds in Rosin by Gas Chromato^aphy...................................................... 06834 Test Method for Composition of Turpentine by Gas Chromatography............................ .......... Spediication for Phthalocyanine Green Pigments.............. -------------------------.......... -- 0683 0682 Test Method for Color and Practice for Determination Strength of Color Pigments by Use ofa Miniature Sandmill of Resistance of Factory-Applied Coatings on Wood Products ........... to Stains and 0682 & M 068f Test Method for Monomethyl Ether of Hydroquinone in Colorless Monomeric Acrylate Esters and 0683 SpedtoCtion"for n-Butyl Acetate (98% Grade) (Discontinued 1987+--Replaced by Specification D4615) - -------* 06831 D 312 D 312 D312 D313 D313 D313 D313 D316 D316 SD 317 D32f D 32f D 32f D32.` D32t D32 D32 D 32 D32 D 32 D32 D'32 "8 : D 3: D 3: D3.' " 3: " 3: D3: D3 D3 D3 D3 D3 D3 D" D - ": ": ": D. ": " : D D D D D D D D D D DUP050297168 CONTENTS, VOLUMES 06.01,06.02, AND 06.03 D 3127 - 83 D 3128-89 D 3129 - 91 D 3130 - 86 D 3131 - 88 D3132-84(1990)I D3133 -72(1989)" D3I68-85(1990)" D 3169 - 89 D 3170 - 87 (199 l)el D3256 - 86 (1991)" D 3257 - 88 D 3258 - 80 (1987)" D 3259 - 84 (1990)" D 3260 - 82 (1991) D 3271 - 87 D 3272 - 76 (1988)" D 3273 - 86 (1991)" D 3274 - 82 (1988)" D 3276 - 86 D 3278 - 89 D 3280 -85(1990)" D 3281 - 84 (1989) D 3322 - 82 (1991) D3323-80(1988)" D3329-89 D3335 -85a" (1991)" D 3358 - 88 D 3359 - 90 D 3360 - 80 (1989) D 3361 - 87 D 3362 - 84 (1987) D 3363 - 74 (1989)" D 3383 - 79a (1988)" D 3424 - 75 D 3425 - 80 (1988)" D 3432 - 89 D 3450 - 90 D 3451-76 (1987)" D 3456 - 86 {1991)" D 3457 -87(1991)" D 3459 - 87 D 3516 - 89 D 3539 - 87 D 3540 - 86 D 3541 - 91 D 3545 - 90 D 3546 - 90 D 3547 - 91 D 3548 - 86 D3618 - 85a(1991)" D 3619 - 77 (1989) D 3620 - 90 D 3621 - 84 D 3622 - 90 D 3623 - 78a (1987) D 3624 - 85a (1991)" Specification for n-Ethyl Acetate (99 % Grade) (Discontinued 1987f--Replaced by Specification D4614) ....................................................................................................................................................... 06.03 Specification for 2-Methoxyethanol ........................................................................................................... 06.03 Guide for Testing Exterior Latex House Paints....................................................................................' `' Q6.01 Specification for n-Propyl Acetate (96 % Grade)...................................................................................... ' q 6_q 3 Specification for Isopropyl Acetate (99 % Grade).......................................................................................... 06.03 Test Method for the Solubility Range of Resins and Polymers.................................................................... 06.02 Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Lacquers by Infrared Spectrophotometry.......................................................................................................................................06411 Practice for the Qualitative Identification of Polymers in Emulsion Paints............................................... 06.01 Specification for Refined Sunflower Oil............. ......................................................................................... 06.03 Test Method for Chipping Resistance of Coatings........................................................................................ 06.01 TestMethods for Chemical Analysis of Phthalocyanine Blue and Green Pigments.....................................06.02 Test Method for Aromatics in Mineral Spirits by Gas Chromatography ....................................................06.03 Test Method for Porosity of Paint Films........................................................................................................ 06.01 Practice for Infrared Determination ofthe Temperature of Applied Coatings on Wood Products During the Curing Cycle...........................................................................................................................................06.01 Test Method for Acid and Mortar Resistance ofFactory-Applied Clear Coatings on Extruded Aluminum Products.........................................................................................................................................................06.01 Practice for Direct Injection of Solvent-Reducible Paints into a Gas Chromatograph for Solvent Analysis.........................................................................................................................................................06.01 Practice for Vacuum Distillation of Solvents from Solvent-Reducible Paints for Analysis....................... 06.01 Test Method for Resistance to Growth ofMold on the Surface ofInterior Coatings in an Environmental Chamber.......................................................................................................................................................06.01 Test Method for Evaluating Degree of Surface Disfigurement of Paint Films by Microbial (Fungal or Algal) Growth or Soil and Dirt Accumulation..........................................................................................06.01 Guide for Painting Inspectors (Metal Substrates).......................................................................................... 06.01 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus........................................... 06.03 Test Methods for Analysis of White Zinc Pigments.......................................................................................064)2 Test Method for Formability of Attached Organic Coatings with Impact-Wedge Bend Apparatus......... 064)1 Practice for Testing Primers and Primer Surfacers Over Preformed Metal ................................................06.01 Guide for Testing Interior Solvent-Reducible Flat Wall Paints.................................................................... 06.01 Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography .............................r..........06.03 Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy................................................................................................................................................ 06.01 Guide for Testing Water-Borne Floor Paints.................................................................................................06.01 Test Methods for Measuring Adhesion by Tape Test......... ..........................................................................06.01 Test Method for Particle Size Distribution By Hydrometer of the Common White Extender Pig ments ............................................................................................................................................................. 06.02 Practice for Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Flame Carbon-Arc . Type) for Testing Paint, Varnish, Lacquer, and Related Products Using the Dew Cycle...................... 06.01 Test Method for Purity of Acrylate Esters by Gas Chromatography............................................................ 06.03 Test Method for Film Hardness by Pencil Test.............................................................. Guide for Testing Solvent-Reducible Floor Paints........................................................................................ 06.01 Method of Evaluating the Lightfastness of Printed Matter............................................................................ 06.01 Guide for Testing Solvent-Reducible Interior Semigloss Wall and Trim Enamels......................................06.01 Test Method for Unreacted Toluene Diisocyanates in Urethane Prepolymers and Coating Solutions by Gas Chromatography.................................................................................... Test Method for Washability Properties of Interior Architectural Coatings............................................... 064)1 Practices for Testing Polymeric Powders and Powder Coatings.................................................................... 06.01 Practice for Determining by Exterior Exposure Tests the Susceptibility ofPaint Films to Microbiological ' Attack ........................................................................................................ Test Method for Preparation of Methyl Esters from Fatty Adds for Determination of Fatty Add Composition by Gas-Liquid Chromatography ..........................................................................................06.03 Test Method for Humid-Dry Cycling for Coatings on Wood and Wood Products....................................06.01 Test Method for Ashing Cellulose................................................................................................................... 06.02 Test Methods for Evaporation Rates of Volatile Liquids by Shell Thin-Film Evaporometer ................... 06.01 Specification for Primary Amyl Acetate, Synthetic (98 % Grade).................................................................06.03 Specification for 2-Ethylhexyl Acrylate ...~i.................................................................................................. 064)3 Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography ....................... 06.03 Test Method for Formic Add in Glacial Acetic Add.....................................................................................06.03 Spedfication for -Butyl Acrylate.................................................................... Specification for Ethyl Acrylate......................-................................................................................................06.03 Test Method for Detection of Lead in Paint and Dried Paint Films............................................................ 06.01 Specification for Aluminum Silicate Pigments (Anhydrous).........................................................................06.02 Specification for Glacial Acetic Acid-...................... .................... ............................. j.............................. 06.03 Practice for Determination of Water in Acetate Esters (Discontinued 1988f--Replaced by Test Method D 1364)................................................................................................... Spedfication for n-Propyl Alcohol (1-Propanol)............................................................................................. 06.03 Method for Testing Antifouling Panels in Shallow Submergence................................................................ 06.01 Test Method for Low Concentrations of Mercury in Paint by Atomic Absorption Spectroscopy ........... 064)1 xvn 06.01 f i DUP050297169 D 3630-89 D 3680-89 D 3717-85a (I99i)" D 3718- 85a <1991)fl D 3719-87 D 3720 - 90 D3721 - 83 (1991)" D3722 - 82 (1991)" D 3723-84 (1990)" D 3724-82 (1987)" 03725-78(1988)" D 3726-84 D 3727 - 84 D 3728 -88 D 3729 -84 D 3730-78 (1988)" 0 3732 - 82(1989)" 0 3733 - 78(1984)" D 3734-91 D 3735-87 D 3792 - 91 D 3793-89 D 3794 - 79" D 3804 - 86 (1991)" D 3806 - 90a D 3842-86 (1991) D 3843-89 D 3845-89 0 3872 - 86(1991)" D 3876-79 (1989)" 03891-90 0 3893 - 90 D39U-89 D 3912 -80 (1989) D 3924-80 (1991)" D 3925-91 D 3926-80 (1991)" D 3927-87 D 3928-89 D 3934 - 90 D3941-90 0 3960 - 91 D 3964 - 80 (1989) D 3969-85 (1990)" D 3970 -80 (1990)" 03971-89 D 3980-88 D 3988-85 (1990)" D 3989 - 81a (1990)" D 4017-90 D 4039-87 D 4040 - 91 D 4060-90 D 4062 - 88 D 4082-89 D4085 - 81 (1987) D4121 -82(1987) 04138 - 88 04139 - 82(1991)" CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 Guide for Determining Constituents Classified as Hazardous Contained in Protective ng Test Method for Residual Vinyl Chloride Monomer Content of Poly(Vinyl Chloride) Resins Compounds, and Copolymers by Solution Injection Technique.......................................... ' 06 02 Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy........06Ai Test Method for Low Concentrations of Chromium in Paint by Atomic Absorption Spectroscopy Test Method for Quantifying Dirt Collection on Coated Exterior Panels................................ 06JM Qg nj Test Method for Ratio of Anatase to Rutile in Titanium Dioxide Pigments by X-Ray Diffraction 06.02 Specification for Synthetic Red Iron Oxide Pigment................................................................ gg Specification for Natural Red and Brown Iron Oxide Pigments..............................................gg Test Method for Pigment Content of Water-Emulsion Paints by Low-Temperature Ashinggg'nt Specification for Synthetic Brown Iron Oxide Pigment...................................................................... 06D2 Test Method for Semiquantitative Determination of Fish Oil in Drying Oils and Drying Oil Fatty Acids by Gas-Liquid Chromatography.......................................................................................................... gg nj Specification for n-Butyl Acetate (99.5 % Grade) (Discontinued 1987f--Replaced by Specification D46I5)..................................................................................................................................................... ... Specification for Ethyl Acetate (99.5 % Grade) (Discontinued 1987t--Replaced by Specification D4614)........................................................................................................................................................ Specification for 2-Ethoxyethyl Acetate (99 % Grade)............................................................................. 06.03 Specification for Methyl Ethyl Ketone (99.5 % Grade) (Discontinued 1989t--Replaced by Specification D 740)....................................................................................................................................................... 054)3 Guide for Testing High-Performance Interior Architectural Wall Coatings........................................... 05.04 Practice for Reporting Cure Times of Ultraviolet-Cured Coatings................................................... \\\ 063)1 Test Method for Silicon Content of Silicone Polymers and Silicone-Modified AUcyds by Atomic Absorption.................................................................................................................................................06.02 Specification for High-Flash Aromatic Naphthas...................................................................................... 06.03 Specification for VM&P Naphthas.......... ................................................................................................. 06.03 Test Method for Water Content of Water-Reducible Paints, by Direct Injection Into a Gas Chromatograph..................................... ...................................................................................................064)1 Test Method for Low-Temperature Coalescence of Latex Paint Films....................................................064)1 Practice for Testing Coil Coatings..............................................................................................................064)1 Test Method for Iron in Paint Driers by EDTA Method......................................................................... 064)3 Test Method for Small-Scale Evaluation of Fire-Retardant Paints (2-Foot Tunnel Method) ................ 064)1 Guide for Selection of Test Methods for Coatings for Use in Light-Water Nuclear Power Plants ........06.01 Practice for Quality Assurance for Protective Coatings Applied to Nuclear Facilities........................... 064)1 Specification for Glacial Methacrylic Acid................................................................................................06.03 Test Method for Ferrous Iron in Iron Oxides.................................. ........................................................06.02 Test Method for Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography...................................................................................................................................... 064)2 Practice for Preparation of Glass Panels for Testing Paint, Varnish, Lacquer, and Related Products... 064)1 Test Method for Purity of Methyl Amyl Ketone and Methyl Isoamyl Ketone by Gas Chromatography 06.03 Test Method for Evaluating Coatings Used in Light-Water Nuclear Power Plants at Simulated Design Basis Accident (DBA) Conditions.......................................................................................................... 064)1 Test Method for Chemical Resistance of Coatings Used in Light-Water Nuclear Power Plants............ 064)1 Specification for Standard Environment for Conditioning and Testing Paint, Varnish, Lacquer, and Related Materials ........................................................................ '........................................................... 864)1 Practice for Sampling Liquid Paints and Related Pigmented Coatings................................................... 064)1 Test Method for Percent Solids in Titanium Dioxide Slurries................................................................. 064)2 Guide for State and Institutional Purchasing of Paint (Intent to Withdraw) ......................................... 064)1 Test Method for Evaluation of Gloss or Sheen Uniformity ...................................................................... 064)1 Test Method for Flash/No Flash Test--Equilibrium Method by a Closed-Cup Apparatus....................06.03 Test Method for Flash Point by the Equilibrium Method with a Closed-Cup Apparatus................ 06.03 Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings. 06.01 Practice for Selection of Coating Specimens for Appearance Measurements..........................................06.01 Test Method for Zirconium in Paint Driers by EDTA Method ............................................................. 06.03 Test Method for Cerium in Paint Driers by Oxidimetric Determination................................................ 06.03 Test Method for Dichloromethane-Soluble Matter in Cellulose............................................................. 064 Practice for Interlaboratory Testing of Paint and Related Materials....................................................... 064)1 Test Method for Vanadium in Paint Driers by EDTA Method... .......................................... Test Method for Total Rare Earth Metals in Paint Dners by EDTA Method ........................................ 0640 Test Method for Water in Paints and Paint Materials by Karl Fischer Method...................................... 06411 Test Method for Reflection Haze of High-Gloss Surfaces ........ ;........................... X? m Test Method for Viscosity of Printing Inks and Vehicles by the FaUmg-Rod Viscometer......................06.01 Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser.................................. 06.01 Test Method for Leveling of Paints by Draw-Down Method.................................. . ........ ................... "?,,* Test Method for Effects of Radiation on Coatings for Use in Light-Water Nuclear Power Plants........ 06.01 Test Method for Metals in Cellulose by Atomic Absorption Spectrophotometty^. ..........................0D4 Practice for Photographic Documentation of Coating and Lining Failures and Defects ... - . 06.01 T^tMethod ^Measurement of Dry Film Thickness of Protective Coating Systems by Destructive ^ Guide for Determining Volatile and Nonvolatile Content of Pigments.................................................. 064)2 D D D D D D D D D D D D D D D D D D D D D D D D D D D D D D D E D E E r r r r 1 ' r E E E E E E E E E E E E E E E ffftiM'JKiiilim DUP050297170 CONTENTS, VOLUMES 06.07, 06.02, AND 06.03 1 D4140 - 82 (1991)" Guide for Determining Volatile and Nonvolatile Content of Driers, Drying Oils, Naval Stores, and Solvents................................................................................................................................ 06.03 2 D 414! - 82 (1987)" Practice for Conducting Accelerated Outdoor Exposure Tests of Coatings.................................................. 06.01 1 D4142 - 89 Guide for Testing Epoxy Resins............................................................................ 06.02 1 D 4143 - 89 Guide for Testing Latex Vehicles..................................................................................................................... 06.02 1 D 4144 _ 82 (1987) Method for Estimating Package Stability of Coatings for Ultraviolet Curing.............................................. 06.01 2 D 4145 - 83 (1990)" Test Method for Coating Flexibility of Prepainted Sheet...............................................................................06.01 2 D 4146 - 83 (1989)" Test Method for Formability of Zinc-Rich Primer/Chromate Complex Coatings on Steel........................06.01 2 D4147 - 82 (1987) Practice for Applying Coil Coatings Using the Wire-Wound Drawdown Bar.............................................. 06.01 I D 4206 - 89 Test Method for Sustained Burning of Liquid Mixtures by the Setaflash Apparatus (Open Cup) 06.01, 06.03 2 D 4207 - 91 Test Method for Sustained Burning of Low-Viscosity Liquid Mixtures by the Wick Test..........................06.03 D4209 - 82 (1991)" Practice for Determining Volatile and Nonvolatile Content of Cellulosics, Emulsions, Resin Solutions, 3 Shellac, and Varnishes................................................................................................................................ 06.02 D 4212 - 88 Test Method for Viscosity by Dip-Type Viscosity Cups................ 06.01 3 D 4213 - 87 D 4214 - 89 Test Method for Wet Abrasion Resistance of Interior Paints ...................................................................... 06.01 Test Methods for Evaluating Degree ofChalking of Exterior Paint Films.................................................. 06.01 3 D4227 - 83 (1989) Practice for Qualification of Journeyman Painters for Application of Coatings to Concrete Surfaces of 3 Safety-Related Areas in Nuclear Facilities..................................................................................................06.01 D4228 - 83 (1989) Practice for Qualification of Journeyman Painters for Application of Coatings to Steel Surfaces of 3 Safety-Related Areas in Nuclear Facilities.............................. 06.01 1 D 4236 - 91 Practice for Labeling Art Materials for Chronic Health Hazards...................................................................06.01 1 D 4256 - 89 Test Method for Determination of the Decontaminability of Coatings Used in Light-Water Nuclear Power Plants.................................................................................................................................................06.01 2 D 4257 - 87 Practice for Design and Use of Safety Alert System for Hazardous Work Locations in the Coatings and 3 Lining Industry (Discontinued 1990f)....................................................................................................... 06.01 3 D 4258 - 83 (1988) Practice for Surface Cleaning Concrete for Coating................................................ 06.01 D 4259-88 Practice for Abrading Concrete....................................................................................................................... 06.01 1 D 4260 - 88 Practice for Acid Etching Concrete........ ......... ;......................................................................................... 06.01 I D 4261 - 83 (1988) Practice for Surfece Cleaning Concrete Unit Masonry for Coating.............................................................. 06.01 1 D 4262 - 83(1988) Test Method for pH of Chemically Cleaned or Etched Concrete Surfaces..................................................06.01 3 D4263 - 83 (1988)" Test Method for Indicating Moisture in Concrete by the Plastic Sheet Method..........................................06.01 1 D 4277 - 83 (1988)" Guide for Testing Amino Resins........................... 06.02 1 D 4285 - 83 (1988) Test Method for Indicating Oil or Water in Compressed Air................... 06.01 1 D 4286 - 90 Practice for Determining Coating Contractor Qualifications for Nuclear Powered Electric Generation 3 Facilities.................................................. 06.01 2 D 4287 - 88 Test Method for High-Shear Viscosity Using the ICI Cone/Plate Viscometer........................................... 06.01 D 4288-83 (1989)" Specification for Calcium Borosilicate Pigments.............................................................................................06.02 2 D 4301 - 84(1989)" Test Method for Total Chlorine in Epoxy Resins:and Compounds............................................................ 06.02 1 D 4302 - 90 Specification for Artists' Oil, Resin-Oil, and Aikyd Paints............................................................................ 06.01 3 D 4303 - 91 Test Methods for Lightfastness of Pigments Used in Artists' Paints ........................................................... 06.01 D 4358 - 84 (1990)" Test Method for Lead and Chromium in Air Particulate Filter Samples ofLead Chromate Type Pigment 1 Dusts by Atomic Absorption Spectroscopy................................................................................................06.02 1 D4359 - 90 Test Method for Determining Whether a Material is a Liquid or a Solid.................................................... 06.01 D4360 - 90 Specification for Methyl n-Amyl Ketone......................................................................................................... 06.03 9 D 4361 - 89 Test Method for Apparent Tack of Printing Inks by the Inkometer.............................................................06.01 9 D 4366 - 91 Test Methods for Hardness of Organic Coatings by Pendulum Damping Tests.......................................... 06.01 D 4367 - 89 Test Method for Benzene in Hydrocarbon Solvents by Gas Chromatography............................................ 06.03 D 4368 - 89 Guide for Testing PoIy(Vinyl Chloride) Resins................................................. ...................................... . 06.02 D 4370. - 84 (1990)" Test Methods for Acid and Base Milliequivalent Content of Electrocoat Bath............................................ 06.01 D 4399 - 90 Test Method for Measuring Electrical Conductivity of Electrocoat Baths.................................................... 06.01 D 4400 - 89a Test Method for Sag Resistance ofPaints Using a Multinotch Applicator,.................................................. 06.01 D4414 _ g4 (1990)" Practice for Measurement of Wet Film Thickness by Notch Gages.............................................................06.01 D 4415 - 91 Test Method for Determination of Dimer in Acrylic Acid.......... .................................................................. 06.03 J D 4416 - 89 Specification for Acrylic Add..........................................................................................................................06.03 3 D 4417 - 84 Test Methods for Field Measurement of Surface Profile ofBlast Cleaned Steel.......................................... 06.01 2 D 4449 - 90 Test Method for Visual Evaluation of Gloss Differences Between Surfaces of Similar Appearance -- 06.01 1 04450 - 85 (1990)" Test Method for Analysis of Zinc Hydroxy,Phosphite Pigment .................................................................. 06.02 3 D4451 - 85 (1991)" Test Method for Pigment Content of Paints by Low-Temperature Ashing.................................................. 06.01 3 D 4457 - 85 (1991)" Test Method for Determination of Dicfaloromethane and H,L-Trichloroethane in Paints and Coatings 1 by Direct Injection into a Gas Chromatograph.......................................................................................... 06.01 1 D 4462 - 85 (1989) Specification for Zinc Hydroxy Phosphite Pigment........;.................... 06.02 I D4487 - 90 Test Methods for Analysis of Caldum Borosilicate ^........ .................................................. 06.02 S D4518 - 91 Test Methods for Measuring Static Friction ofCoating.Surfaces...................... 06.01 1 D4537 - 91 Guide for Establishing .Procedures to Qualify and Certify Inspection Personnel for Coating Work in 1 Nuclear Facilities...... ......................................... ;..............;................ ...........:.......................................06.01 2 D 4538 - 90a Terminology Relating to Protective Coating,and Lining Work for Power Generation Facilities.......... 06.01 1 D 4540 - 91 Guide for Testing Interior Latex Semigloss and Gloss Paints.................. 06.01 D4541 - 85 (1989)" Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers ...................................... 06.01 1 D4563 - 86 (1991)" Test Method for Determination by Atomic Absorption Spectroscopy of Titanium Dioxide Content of 2 Pigments Recovered from Whole Paint.............................................................................................. 06.01 D4584 - 86(1991)" Test Method for Measuring Apparent pH ofElectrocoat Baths ................................................................... 06.01 xix DUP050297171 D 4585-87" D 4587-91 D4610-86 D4613 - 86 (1990)" D4614 - 86 D4615 - 86" D 4618-87 D4619-91 D4639 - 86 (1990)" D4640 - 86 (1990)" D 4706-87 D4707-87 D4708-91 D 4709-87 D 4710-87 D 4712-87a (1991) D 4713-87" D 4747 - 87 D 4752 -87 0 4758 - 87 D 4764-88 D 4773-89 D 4787 - 88 D 4794-88 D 4795 -88 D 4796 - 88 D 4797-88 D 4827-88 D4828 - 91 D 4834-88 D 4835- 89 D 4836 - 90 D 4837 - 89 D 4838-88 D 4938-89 D 4939-89 D 4940-89 D 4941-89 D 4942-89 D 4946 - 89" D 4948-89 D 4958-91 D 4960 - 89 D5007 - 89 D 5008-89 0 5009 - 89 05010-91 0 5031-89 D 5043 - 90 0 5062 - 90" 0 5063 - 90 0 5064 - 90 0 5065 - 90 0 5066 - 91 0 5067 - 90" 05068-90 0 5069 - 90 CONTENTS, VOLUMES 06.01,06.02, AND 06.03 Practice for Testing Water Resistance of Coatings Using Controlled Condensation.................................06.01 Practice for Conducting Tests on Paint and Related Coatings and Materials Using a Fluorescent UV-Condensation Light- and Water-Exposure Apparatus..................................................................... 06.01 Guide for Determining the Presence of and Removing Microbial (Fungal or Algal) Growth on Paint and Related Coatings.......................................................................................................................................... 06.01 Test Method for Measuring Apparent pH of Water Insoluble Phenol-Formaldehyde Resins.................. 06.02 Specification for Ethyl Acetate (All Grades)..................................................................................................06.03 Specification for -Butyl Acetate (All Grades) ..................................................................... 06.03 Specification for Design and Fabrication ofFlue Gas Desulfurization System Components for Protective Lining Application...................................................................................................................................... 06.01 Practice for Inspection of Linings in Operating Flue Gas Desulfurization Systems................................ 06.01 Test Method for Volatile Content in Phenolic Resins................................................................................. 06.02 Test Method for Determining Stroke Cure Time of Thermosetting Phenol-Formaldehyde Resins........ 06.02 Test Method for Determining Qualitatively Methylol Group in Phenolic Resins .................................... 06.02 Test Method for Measuring Paint Spatter Resistance to Roller Application...............................................06.01 Practice for Preparation of Uniform Free Films of Organic Coatings.......................................................06.01 Specification for Methyl Acrylate .......................................:.......................................................................06.03 Specification for Acetaldehyde................................................ 06.03 Guide for Testing Industrie Water-Reducible Coatings....................................................................... -- 06.01 Test Methods for Nonvolatile Content of Printing Inks, Resin Solutions, and Vehicles........................ 06.01 Test Method for Determining Unreacted Monomer Content of Latexes Using Gas Chromatography.. 06.02 Test Method for Measuring MEK Resistance of Ethyl Silicate (Inoiganic) Zinc-Rich Primers by Solvent Rub...............................................................................................................................................................06.01 Test Method for Nonvolatile Content of Latexes.................... 06.02 Test Method for Determination by X-ray Fluorescence Spectroscopy of Titanium Dioxide Content in Paint ............................................................................................................................................................ 06.01 Test Method for Purity of Propylene Glycol Monomethyl Ether, Dipropylene Glycol Monomethyl Ether, and Propylene GlycolMonomethyl Ether Acetate ............... 06.03 Practice for Continuity Verification of Liquid or Sheet Linings Applied to Concrete Substrates.......... 06.01 Test Method for Determination of Ethoxyl Substitution in Cellulose Ether Products by Gas Chromatography................................. ................................................................................................... 06.02 Test Method for Nitrogen Content of Soluble Nitrocellulose--Alternative Method..............................06.02 Test Method for Bond Strength of Thermoplastic Traffic Marking Materials'........................................ 06.01 Test Methods for Chemical and Gravimetric Analysis of White and Yellow. Thermoplastic Marking Containing Lead Chromate and Titanium Dioxide...............................................................................06.01 Test Method for Determining the Unreacted Monomer Content of Latexes Using Capillary Column Gas Chromatography...............................'....................................................................................................... 06.02 Test Method for Practical Washability of Organic Coatings .................................................................... 06.01 Test Method for Detection of Lead in Paint by Direct Aspiration Atomic Absorption Spectroscopy... 06.01 Specification for Propylene Glycol Monomethyl Ether Acetate .............................................................. 064)3 Specification for Dipropylene Glycol Monomethyl Ether........................................................................ 064)3 Specification for Propylene Glycol Monomethyl Ether............................................................................ 064)3 Test Method for Determining the Relative Tinting Strength of Chromatic Paints.................................. 064)1 Test Method for Erosion Testing of Antifouling Paints Using High Velocity Water.............................. 064)1 Test Method for Subjecting Marine Antifouling Coating to Biofouling and Fluid Shear Forces in Natural Seawater 064)1 Test Method for Conductimetric Analysis of Water Soluble Ionid Contamination of Blasting Abrasives. 064)1 Practice for Preparing Drawdowns of Artists-' Paste Paints ,........................ ............................. ............ 064)1 Test Methods for Water Pickup of Lithographic Printing Inks and Vehicles in a Laboratory Mixer ... 064)1 Test Method for Blocking Resistance of Architectural Paints............................ ..................................... 064)1 Test Method for Determination of the Upper Layer Separated from a Viscous Liquid .................. . 064)1 Test Method for Comparision of the Brush Drag of Latex Paints .................. .. .................................... 064)1 Test Method for Evaluation of Color for Thermoplastic Traffic Marking Materials.............................. 06.01 Test Method for Wet-to-Dry Hiding Change........ i................................................................................ 06.01 Test Method for Ethyl Methyl Pentanol Content and Purity Value of 2-Ethylhexanol by Gas Chromatography ............................ .................................................................................. ..................... 06.03 Test Method for Evaluating and Comparing Transfer Efficiency Under Laboratory Conditions.......... 06.01 Guide for Testing Printing Inks and Related Materials ........................ :'........................................ 064)1 Practice for Conducting Tests on Paintsand Related Coatings and Materials Using Enclosed Carbon-Arc light and Water Exposure Apparatus................................ '......................................................... 06.01 Test Methods for Field Identification of Coatings ................................ ....................................... 064)1 Test Method for Resin Solution Dilutability. -.. ...................................... .......................................... 06.01 Guide for Use of Certification ofCoating Conformance Form ... ........ .............................................. 064)1 Practice for Conducting a Patch Test to Assess Coating Compatibility.................................................... 06.01 Guide for Assessing the Condition of Aged Coatings on Steel Surfaces .......................... 06.01 Test Method for Determination of the Transfer Efficiency Under Production Conditions for Spray Application of Automotive Paints--Weight Basis............ . '.............. .................................................. 06.01 Specification for Artists' Watereolor Paints.............. - - . *-.r,i .................... ........................................... 06.01 Practice for Preparation of Paint Brushes for Evaluation.';..;....................................... r 064)1 Practice for Preparation of Paint Roller Covers for Evaluation........ ....................................................... 064)1 f : i '} i xx DUP050297172 1 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 D 5087 - 91 D 5095 - 90 D 5097 - 90 D 5098 - 90 D 5107 - 90 D 5108 - 90 D 5125 - 91 D 5137 - 90 D 5139 - 90 D 5144 - 91 D 5145 - 90 D 5146 - 90 D 5150 - 91 D 5161 - 91 D 5162-91 D 5163 -91 D 5164 - 91 D 5166 - 91 D 5178 - 91 D 5179-91 D 5181 - 91 D 5200 - 91 D 5201 - 91 E 28 - 67 (1982)" E 97-82 (1987) E 259 - 91 E 430-91 E 852 - 82 (1987)" G 6-88 G 8-90 G 9-87 G10-83 (1988) G 11-88 G12-83 (1988) G 13-89 G 14-88 G 17-88 G 18-88 G 19-88 G 20-88 G 23-90 G 26-90 G 42-90 G 53-88 Test Method for Determining Amount of Volatile Organic Compound (VOC) Released from Automotive Coatings and Available for Abatement............................................................................... 06.01 Test Method for Determination of the Nonvolatile Content in,Silanes, Siloxanes, and Silane-Siloxane Blends Used in Masonry Water Repellant Treatments.......... '............................................................. . 06.01 Test Method for Filter-Retained Solids Content of Polymer Latexes........................................................ 06.02 Specification for Artists' Acrylic Emulsion Paints ......................................................................................... 06.01 Practice for Preparatory Surface Cleaning of Architectural Sandstone.......................................... 06.01 Test Method for Organotin Release Rates ofAntifouling Coating Systems in Sea Water.......................... 06.01 Test Method for Viscosity of Paints and Related Materials by ISO Flow Cups.......................................... 06.03 Specification for Hexyl Acetate........................................................................................................................06.03 Specification for Sample Preparation for Qualification Testing ofCoatings to be Used in Nuclear Power Plants.............................................................................................................................................................06.01 Guide for the Use of Protective Coating Standards in Nuclear Power Plants.............................................. 06.01 Test Method for Nonvolatile and Pigment Content of Electrocoat Baths.................................................... 06.01 Guide to Testing Solvent-Borne Architectural Coatings.................................................................................06.01 Test Method for Hiding Power of Architectural Paints Applied by Roller.................................................. 06.01 Guide for Specifying Inspection Requirements for Coating and lining Work (MetalSubstrates).............06.01 Practice for Discontinuity (Holiday) Testing of Nonconductive Protective Coating on Metallic Substrates.......................................................................................................................................................06.01 Guide for Establishing Procedures to Monitor the Performance of Safety Related Coatings in an Operating Nuclear Power Plant...............................................................................................................06.01 Specification for Propylene Glycol and Dipropylene Glycol.........................................................................06.03 Practice for the Laboratory Preparation of Gelled Vehicle Samples Usinga Microwave Oven.................06.02 Test Method for Mar Resistance of Organic Coatings...................................................................................06.01 Test Method for Measuring Adhesion of Organic Coatings to Plastic Substrates by Direct Tensile Testing......................................................................................... 06.01 Test Method for Abrasion Resistance of Printed Matter by the GA-CAT Comprehensive Abrasion ... 06.01 Test Method for the Determination ofVolatile Organic Compounds (VOC) of Solvent Reducible Paints in Aerosol Cans........................ 06.01 Practice for Calculating Formulation Physical Constants of Paints and Coatings ......................................06.01 Test Method for Softening Point by Ring-and-Ball Apparatus.................................................................... 06.03 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry...................................................................................................................... 06.01 Practice for Preparation of Reference White Reflectance Standards .......................................................... 06.01 Method for Measurement of Gloss of High-Gloss Surfaces By Goniophotometry ....................................06.01 Test Methods for C4-C13 Plasticizer Grade Alcohols.................................................................................... 06.03 Test Method for Abrasion Resistance of Pipeline Coatings ........................................................................ 06.01 Test Methods for Cathodic Disbonding of Pipeline Coatings...................................................................... 06.01 Test Method for Water Penetration Into Pipeline Coatings.......................................................................... 06.01 Test Method for Specific Bendability of Pipeline Coatings.......................................................................... 06.01 Test Method for Effects of Outdoor Weathering on Pipeline Coatings ....................................................... 06.01 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings an Steel.......... 06.01 Test Method for Impact Resistance of Pipeline Coatings (Limestone Drop Test)..................................... 06.01 Test Method for Impact Resistance of Pipeline Coatings (Falling Weight Test)..........................................06.01 Test Method for Penetration Resistance of Pipeline Coatings (Blunt Rod) ................................................06.01 Test Method for Joints, Fittings, and Patches in Coated'Pipelines.............................................................. 06.01 Test Method for Disbonding Characteristics of Pipeline Coatings by Direct Soil Burial........................... 06.01 Test Method for Chemical Resistance of Pipeline Coatings.......................................................................... 06.01 Practice for Operating Light-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Exposure of Nonmetallic Materials .......................... 06.01 Practice for Operating Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of Nonmetallic Materials.................................. 06.01 Method for Cathodic Disbonding of Pipeline Coatings Subjected to Elevated Temperatures................... 06.01 Practice for Operating Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for Exposure of Nonmetallic Materials............................................................................................... 06.01 AROMATIC HYDROCARBONS AND RELATED CHEMICALS (see gray-edged pages 539 to 817 of Volume 06.03) i D 362 - 84 Specification for Industrial Grade Toluene (Discontinued 1991)........................... 06.03 i D 835 - 90 Specification for Refined Benzene-485 ..................... 06.03 l D 836 - 84 Specification for Industrial Grade Benzene (Discontinued 1991).............................................................. 06.03 l D 841 - 90 Specification for Nitration Grade Toluene............. .................................... 06.03 l D 843 - 90 Specification for Nitration Grade Xylene .................................................................................................... 06.03 D 846 - 84 Specification for Ten-Degree Xylene (Discontinued 1991)...................................................................... 06.03 t D 847-91 Test Method for Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial l Aromatic Hydrocarbons ............ ...................................... .......................................................................06.03 I D 848-81 (1989)" Test Method for Acid Wash Color of Industrial Aromatic Hydrocarbons..................................................06.03 t D 849-88 Test Method for Copper Corrosion of Industrial Aromatic Hydrocarbons ..................... 06.03 D 850-91 Test Method for Distillarion of Industrial Aromatic Hydrocarbons and Related Materials ..................... 06.03 DUP050297173 852 -87(1991) 853 -91 D 1015 -84 D 1016 -84 D 1492 -91 D 1493 -90 D 1555 -91 D 1631 - 85 (1989)" 0 1685 -86(1990) D 1686 -81(1990) D 2030 84(1989)" D2031 -84(1989)" D2H9 -87 D2120- -87 0=2121 -90 D 2232 - 81 (1986)" D 2306 - 81(1985) D 2323 -84(1989)" D 2324 -81 (1989)" D2340- -82(1987)" D2359- 90 D 2360 -82(1987)" D2403- -91 D 2439 -91 D 2747 -81 D 2748 - 82 D2827 - 88e D 2870 D 2930 D 2935 D3054D3055D 3160 D3193D 3264 D 3366 - 0 3436 - 91 03437- 89 D 3438 - 89 D 3439 - 89 D 3504 - 91 D 3505 - 91 D 3626 - 85(1990)" D 3627 - 91 D 3760 - 79(1984) D 3797 - 88 D 3798 - 89 D 3799 - 89 D 3852 - 90 D 3961 - 89. D 3962 - 80(1989)" D4076- 86(1990) 04077- 91 D 4297 - 89 D4471 -85(1989)" D 4492 - 85(1989)" 04493- 89 04534- 89 04588- 87 0 4589- 91 04590-86 04734- 90 04735 --87(1991)" D4789--88 CONTENTS, VOLUMES 06.0t, 06.02, AND 06.03 Test Method for Solidification Point of Benzene ..................................................................................... 06.03 Test Method for Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons............................................................................................................................................ 06.03 Test Method for freezing Point of High-Purity Hydrocarbons ................................................................... 06.03 Test Method for Purity of Hydrocarbons from Freezing Points................................................................. 06.03 Test Method for Bromine Index of Aromatic Hydrocarbons by Couloraetric Titration...........................06.03 Test Method for Solidification Point of Industrial Organic Chemicals ..................................................... 06.03 Method for Calculation of Volume and Weight of Industrial Aromatic Hydrocarbons .........................06.03 Test Method for Water in Phenol and Related Materials by the Iodine Reagent Method ...................... 06.03 Test Method for Traces of Thiophene in Benzene by Spectrophotometry................................................. 06.03 Test Method for Color of Solid Aromatic Hydrocarbons and Related Materials in the Molten State (Platinum-Cobalt Scale).............................................................................................................................. 06.03 Test Method for Water Solubility of Refined Pyridine ..............................................................................06.03 Test Method for Reducing Substances in Refined Pyridine ..................................................................... 06.03 Test Method for Aldehydes in Styrene Monomer ........................................................................................06.03 Test Method for Inhibitor, p-rerf-Butylcatechol, in Styrene Monomer ..................................................... 06.03 Test Method for Polymer Content of Styrene Monomer ........................................................................... 06.03 Test Method for Evaporating Residue of Naphthalene................................................................................06.03 Method for Xylene Isomer Analysis by Gas Chromatography ................................................................. 06.03 Specification for Refined Pyridine (I Degree) ................ 06.03 Test Method for Carbon Disulfide in Benzene ............. ............................................................................06.03 Test Method for Peroxides in Styrene Monomer ............ ,...................................................................... 06.03 Specification for Refined Benzene-535 ........................................................................................................ 06.03 Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography .. 06.03 Specification for Refined Phthalic Anhydride-1308 .................................................................................. 06.03 Specification for Refined Phenol ..................................................................................................................064)3 Test Method for Trace Quantities of Total Sulfur in Volatile Organic Liquids (Oxy-Hydrogeo Combustion Methods) (Discontinued 1987f) ....................................................................................... 064)3 Test Method for Pyridine Bases in Tar Acids (Discontinued 1987f--Replaced by Test Method D4471)......................................................... 06.03 Specification for Styrene Monomer 996 ...................................................................................................... 064)3 Test Method for Gel Time of Tar Acids ............................................................... 064)3 Test Method for Maleic Acid in Maleic Anhydride by Potentiometric Titration .................. 06.03 Test Method for Apparent Density of Industrial Aromatic Hydrocarbons ...............................................06.03 Test Method for Purity and Benzene Content of Cyclohexane by Gas Chromatography........................ 06.03 Specification for Cyclohexane 995 .............................................................................................................. 06.03 Test Method for Phenol Content of Isopropylbenzene (Cumene) ...........................................................06.03 Specification for Ethylbenzene ...................................................................................................................... 06.03 Specification for Industrial Grade Aniline .......... ............ .................................................................. 064)3 Test Method for Color of Maleic Anhydride and Phthalic Anhydride in the Molten State and After Heating (Platinum-Cobalt Scale).......... ............ 06.03 Practice for Sampling and Handling Aniline ........................ 06.03 Practice for Sampling and Handling Liquid Cyclic Products .....................................................................06.03 Practice for Sampling and Handling Naphthalene, Maleic Anhydride, and Phthalic Anhydride .......... 064)3 Test Methods for Assay of Alkaline Cresylate Solutions from Petroleum Sources ................................ 06.03 Specification for Maleic Anhydride ............................................................................................................. 06.03 Test Method for Density or Relative Density of Pure Liquid Chemicals...................................................06.03 Test Method for Tar Acid Composition by Gas-Liquid Chromatography.-................................................ 96.03 Test Method for Color of Cresylic Acids ("C" Series Standards) ............................................................... 06.03 Method for Analysis of Isopropylbenzene (Cumene) by Gas Chromatography...................................... 06.03 Test Method for Analysis of o-Xylene by Gas Chromatography ............................................................. 064)3 Test Method for Analysis of p-Xylene by Gas Chromatography .............................................................. 06.03 Test Method for Purity of Styrene by Freezing Point Method .................................................................06.03 Practice for Sampling and Handling Phenol and Cresylic Acid ............ ......... .................................. 06.03 Test Method for Trace Quantities of Sulfur in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry ........................................................................................................................................00-03 Test Method for Analysis of Styrene by Gas Chromatography.......... ..................... ................................ 0603 Specification for o-Xylene 950 ................................... 0603 Specification for Isopropylbenzene (Cumene)................ 06.03 Practice for Sampling and Handling 4,4'-Isopropylidenediphenol (Bisphenol A).................................... 06.03 Test Method for Pyridine Bases in Cresylic Acid by Direct Titration................ ...................................... 06.03- Test Method for Analysis of Benzene by Gas Chromatography ................................................................ 06.03 Test Method for Solidification Point of 4,4'-Isopropylidenediphenol (Bisphenol A).............................. 06413 Test Method for Benzene Content of Cyclic Products by Gas Chromatography............................ .. 064)3 Guide for Analysis ofp-Xylene (Discontinued 1992f--Replaced by Specification D 5136).................. 064)3 Test Method for Nitrobenzene in Aniline......... :............................. .................................................. DW} Test Method for Colorimetric Determination ofp-lert-Butylcatechol in Styrene Monomer by Addition f of Alcoholic NaOH................................................................................................................................... j*:' _ Specification for Refined Benzene-545 ........................ ...: -........................ .......................................... Test Method for Determination of Trace Thiopene in Refined Benzene by Gas Chromatography .... 064M Test Method for Solution Color of 4,4'-Isapropylidenediphenol (Bisphenol A)............................... 06JP- xxu Li Lif Lis M DI Ini AS Re 1 1 1 Ne I I DUP050297174 CONTENTS, VOLUMES 06.01, 06.02, AND 06.03 3 D 4790 - 89a D 4961 - 89 Terminology of Aromatic Hydrocarbons and Related Chemicals................................................................06.03 Test Methods for Gas Chromatographic Analysis of Major Organic Impurities in Phenol Produced; by 3 3 3 3 3 3 3 3 D 5060 - 90 D 5135 - 90 D 5136 - 90 D5194-91 D 5211 - 91 E 299 - 90 E 300 - 86 E 691 -87 the Cumene Process................................................................. .. .t................................................ (fiB Test Method for Determining Impurities in High-Purity Ethylbenzene-byGas Chromatography ...;. 06.03 Test Methods for Analysis of Styrene by Capillary Gas Chromatography.:................................. 06.03 Specification for Purity p-Xylene.....................................................................................................................06.03 Test Method for Trace Chloride in Liquid Aromatic Hydrocarbons............................................................06.03 Specification for Xylene for p-Xylene Feedstock.......................................................................................... 06.03 Test Method for Trace Amounts of Peroxides in Organic Solvents..............................................................06.03 Practice for Sampling Industrial Chemicals...... .. ... ............-.................................................................. 06.03 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method...........06.03 3 RELATED MATERIAL 3 3 . VOLUME, PAGE 3 List by Subjects, Volume 06.01 .................................................................................................... 06.01 xxiv, 06.02 519, 06.03 821 3 List by Subjects, Volume 06.02 ................................................. 06.01 1095, 06.02 xxiv, 06.03 829 3 List by Subjects, Volume 06.03 .... I......................... 06.01 1100, 06.02 527, 06.03 xxiv 3 Metric Practice (Excerpts) (E 380) .........................................!...............,K ...... ............. 06.01 1107,06.02 534, 06.03 835 3 D1 Index........................................................................................................................................... 06.01 1120,06.02 547, 06.03 848 3 Index ........................................................................................V.........................06.01 1133, 06.02 561, 06.03 861 3 ASTM Membership Application 3 3 PENDING STANDARDS ACTION 3 3 3 The following standards action was on Society ballot when this edition,went to press. Ifapproved, the action will be noted in Standardization News and the document will be available soon thereafter as a separate reprint. 3 Revision ofStandards: D 1492-91 3 D 3359-91 3 D4417-91 3 3 New Standards: .. 3 D5165-91 Practice for the Laboratory Preparation of Gelled Vehicles Using a Resin Kettle....................... -- 06.02 3 D 5180 - 91 Test Method for Quantitative Test for Turbidity in Clear Liquids.......................................................... 06.02 3 3 3 3 3 3 3 3 ..in:3 3 i 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 XXU1 DUP050297175 List by Subjects 1992 ANNUAL BOOK OF ASTM STANDARDS, VOLUME 06.01 P < 9:--T' ;<; E => F?@9 AG B' " PCD"E( FG H " II J K L MA CG < ' " <{ Since the standards in this book are arranged in alphanumerical sequence, no page numbers are given in this list. The standards listed in italics are related documents inrinH<vj for information only and do not appear in this volume. For List by Subjects of Volume 06.02 and 06.03, see pp. 1095 and 1100 A complete Subject Index begins on p. 1133 Specificationsfor: D 5098-90 D 4302-90 D 5067 - 90" Test Methodsfor D 969-85 (1989)" D 4399-90 D 1210-79 (1988)" D 1316-87 D 2243-90 D 2337-84 D 3793-89 D 2574-86 D 185 - 84(1989)" D 5062-90" D 869-85(1989)" D 1309-88 04144 - 82(1987) 0 1849 - 80(1987)" D 4948-89 Practicefor D 3925 - 91 Test Methodsfor: D 4958 - 91 D 2353-83 D 2801-69 (1981)" D 4062 -88 D 4400 - 89a 0 2376 - 84(1989) D 4707 - 87 Practicefor D 4941-89 PAINT AND RELATED COATINGS--AS LIQUIDS Artists' Acrylic Emulsion Paints Artists' Paints; Oil, Resin-Oil, and Alkyd Paints Artists' Watercolor Paints Physical Tests General Test Methods Bleeding of Traffic Paint, Determination of Degree of Electrical Conductivity of Electrocoat Baths, Measuring Fineness of Dispersion of Pigment-Vehicle Systems Fineness of Grind ofPrinting Inks by the NPIRI Grindometer Freeze-Thaw Resistance of Water-Borne Coatings Freeze-Thaw Stability of Multicolor Lacquers Low-Temperature Coalescence of Latex Paint Films Microorganisms, Resistance of Emulsion Paints to Attack in the Container Particles, Coarse, in Pigments, Pastes, and Paints Resin Solution, Dilutability Settling of Paint, Evaluating Degree of Settling Properties of Traffic Paints During Storage Stability, Package, of Coatings for Ultraviolet Curing, Estimating Stability, Package, of Paint Upper Layer Separated from a Viscous Liquid, Determination of Sampling Liquid Paints and Related Pigmented Coatings Application Properties Brush Drag of Latex Paints, Comparison of Flow Ratings of Organic Coatings Using the Shell Flow Comparator (Discontinued 1992f) Leveling Characteristics of Paints by Draw-Down Method (Discontinued 1990f) Leveling of Paints by Draw-Down Method Sag Resistance of Paints Using a Multinotch Applicator Slump of Face Glazing and Bedding Compounds on Metal Sash Spatter Resistance to Roller Application, Measuring Preparing Drawdowns of Artists' Paste Paints Approved for use by agencies of the Department of Defense and. if indicated on the standard, replaces corresponding Federal or Military document Const* the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department of Defense. t Although this standard has been officially withdrawn from Society approval, a brief descnpboa is included for information only. XXXV Test Met D 120* I" 154` s D483 D 209t Test Met D 147 Test Me. D 56 D 435' SD219' D421 D428 SD 120 D404 D 154 Test Me D 269 D 514 D 509 D471 D 164 Guidefc D283 Test Me D445 D237 D26S D377 Test Mt D23t D 52( D 501 k Practice D 396 * Test Mt D37S D401 D49^ Test Mt D 16" k s. DUP050297176 Test Methodsfor: D 1209-84(1988)" D 1544 - 80 (1989)" D 4838 - 88 D 2090 -88 Test Methodfor: D 1475 -90 Test Methodsfor: D 562-81 (1990)" D 4359-90 D2196-86(1991)1 D 4212-88 D 4287-88 D 1200 - 88 D 4040 - 91 D 1545-89 Test Methodsfor: D 2697 - 86 D 5145-90 D 5095-90 D 4713 - 87" D1644 - 88 Guide for: D2832-83 (1991)1 Test Methodsfor: D4451 -85 (1991)" D2371 -85 (1990)" D 2698-90 D 3723-84 (1990)" Test Methodsfor: 0 2369 - 90 D 5200 - 91 D 5087-91 Practicefor: 0 3960 - 91 Test Methodsfor: D 3792-91 D4017-90 D 4942 - 89 Test Methodsfor: D 1639-90 LIST BY SUBJECTS, VOLUME 06.01 Color and Clarity ofLiquids Color of Clear Liquids (Platinum-Cobalt Scale) Color of Transparent Liquids (Gardner Color Scale) Tinting Strength, Relative, of Chromatic Paints, Determining Clarity and Cleanliness ofPaint and Ink Liquids (see Vols 06.02, 06.03) Density, Specific Gravity, and Weight per Gallon Density of Paint, Varnish, Lacquer, and Related Products Consistency and Viscosity Consistency of Paints Using the Stormer Viscometer Determining Whether a Material is a Liquid or a Solid Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield) Viscometer Viscosity by Dip-Type Cups Viscosity, High-Shear, Using ICI Cone/Plate Viscometer Viscosity by Ford Viscosity Cup Viscosity of Printing Inks and Vehicles by the Falling-Rod Viscometer Viscosity of Transparent Liquids by Bubble Time Method Analytical Tests Nonvolatile Content Clear or Pigmented Coatings, Volume Nonvolatile Nonvolatile and Pigment Content of Electrocoat Baths Nonvolatile Content in Silanes, Siloxanes, and Silane-Siloxane Blends Used in Masonry Water Repellant Treatments, Determination of Printing Inks, Resins Solutions, and Vehicles Varnishes Paint and Related Coatings Pigment Content Paints by Low-Temperature Ashing Solvent-Reducible Paints Solvent-Reducible Paints Using High-Speed Centrifuge Water-Reducible Paints by Low-Temperature Ashing Volatile Content Coatings Volatile Organic Compounds of Solvent Reducible Paints in Aerosol Cans Volatile Organic Compound (VOC) Released from Automotive Coatings and Available for Abatement, Determining Amount .of Paints and Related Coatings, Volatile Organic Content (VOC) Water Content Water-Reducible Paints by Direct Injection Into a Gas Chromatograph Paints and Paint Materials by Karl Fischer Method ' Water Pickup of Lithographic Printing Inks and Vehicles in a Laboratory Mixer Acid Value and Reactivity Acid Value of Organic Coating Materials XXV DUP050297177 Test Methodsfor: D4370 84(1990)" D2348 91 D3133 72(1989)" D3718 85a D4437 85(1991)" D2621 87 D 3335 85a (1991)" D3618 85a (1991)" D4834 gg D3624 85a (1991)" D4584 86(1991)" D 1542 60(1988)" D2349 90 D4764 88 D4563 86(1991)" D2921 88 D3432 89 Practicesfor: D 3271-87 03168 - 85(1990)" D 2372- 85 (1990)" 0 2743 - 68(1987) D 3272 - 76 (1988)" Guide for: D 1978-91 Test Methodsfor: D 215-91 Specification for: D 358-83(1988) Test Methodsfor: D 4940-89 D 1734 - 63(1980)" D 4262 - 83 (1988) D 2201-65 (1987)" D 4417-84 D 609 - 90 D 2200 - 91 Practicesfor: D 1730 - 67 (1984)" D 1731-67(1984)" D 5107-90 D 4259 -88 D 4260 - 88 D 4258-83 (1988) D4261-83(1988) D 3891-90 D 1732-67(1984) D 2092 - 86 Guide for: D 4610-86 Test Methodsfor: D 823-91 D 1212-91 LIST BY SUBJECTS, VOLUME 06.01 Miscellaneous Methods ofAnalysis Acid and Base Milliequivalent Content of Electrocoat Bath Arsenic in Paint Cellulose Nitrate in Alkyd Lacquers by Infrared Spectrophotometry, Quantitative Determination of Chromium in Paint by Atomic Absorption Spectroscopy, Low Concentrations of Dichloromethane and 1,1,1-Trichloroethane, Analysis for by Direct Injection into a Gas Chromatograph Infrared Identification of Vehicle Solids from Solvent-Reducible Paints Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy, Low Concentrations of Lead in Paint and Dried Paint Films, Detection of Lead in Paint by Direct Aspiration Atomic Absorption Spectroscopy, Detection of Mercury in Paint, Low Concentrations of, by Atomic Absorption Spectroscopy pH, Measuring Apparent, of Electrocoat Baths Rosin in Varnishes, Qualitative Detection of Thinner in Solvent-Reducible Paints, Qualitative Determination of Nature Titanium Dioxide Content in Paint by X-ray.Fluorescence Spectroscopy, Determination of Titanium Dioxide Content of Pigments Recovered from Whole Paint, by Atomic Absorption Spectroscopy Water Repellents and Preservatives in Wood Products, Qualitative Tests for the Presence of Free Toluene Diisocyanates in Urethane Prepolymers and Coating Solutions by Gas Chromatography (see Vol 06.02) Te # I I I I Pn I I r Direct Injection of Solvent-Reducible Paints into a Gas Chromatograph Polymers in Emulsion Paints, Qualitative Identification of Separation of Vehicle from Solvent-Reducible Paints Uniformity of Traffic Paint Vehicle Solids by Spectroscopy and Gas Chromatography Vacuum Distillation of Solvents from Solvent-Reducible Paints for Analysis Te: l Analysis of Electrocoat Bath Samples Systematic Analysis White Linseed Oil Paints, Chemical Analysis of Panel Specifications and Preparation of Surfaces for Painting Wood Panels for Weathering Tests of Coatings Blasting Abrasives, Analysis of Water Soluble Ionic Contamination, Conductimetric Analysis of Concrete and Masonry Panels, Preparation for Paint Testing Concrete Surfaces, pH of Chemically Cleaned or Etched Galvanized Steel Panels, Hot-Dipped Nonpassivated, Preparation for Paint Testing Steel, Blast Cleaned, Field Measurement of Surface Profile Steel Panels, Preparation for Paint Testing Steel Surfaces, Pictorial Surface Preparation Standards for Painting Aluminum and Aluminum-Alloy Surfaces, Preparation for Painting Aluminum Surfaces, Hot-Dip, Preparation for Painting Architectural Sandstone, Preparatory Surface Cleaning of Concrete, Abrading Concrete, Acid Etching Concrete, Surface Cleaning for Coating Concrete Unit Masonry, Surface Cleaning for Coating Glass Panels, Preparation for Testing Paint and Related Products Magnesium Alloy Surfaces, Preparation for Painting Zinc-Coated (Galvanized) Steel Surfaces, Preparation for Painting Microbial (Fungal or Algal) Growth, Determining Presence Film Preparation Tes C t E i Pro C Te l I I I E r E 1D D D D D E Pro: E D Test DUP050297178 Practices for: D4147 - 82 (1987) D4414 - 84 (1990)" D 4708-91 test Methodsfor: $D 1640-83 (1989)" D 1643-60(1988) D 3793 - 89 D 711-89 D 4752 - 87 Practices for: D 3732- 82 (1989)" D 3259-84 (1990)" D 2454-91 Test Methodsfor: D4138-88 D 1186-87 D 1400-87 SD 1005 - 84 (1990)" D 2691-88 G 12-83(1988) Test Methodsfor: D 2065-91 D 3258-80 (1987)" D 1653 -9 la E 96-90 Practicefor: D5162-91 Test Methodsfor: E 97-82(1987) D 3928 - 89 0 4449 - 90 E 430-91 D 523-89 D 5150-91 D 2805-88 D 344-89 D 2064-91 D 4039-87 D 5007 - 89 E 306-71(1976,)" Practicesfor E 259 - 91 D 3964 - 80 (1989) Test Methodsfor: D 969 - 85 (1989)" D 2244 - 89 D 1543 - 86 LIST BY SUBJECTS, VOLUME 06.01 Applying Coil Coatings Using the Wire-Wound Drawdown Bar Thickness, Wet Film, Measurement by Notch Gages Uniform Free Films of Organic Coatings Drying and Caring Drying Times of Organic Coatings at Room Temperature Gas Checking and Draft Resistance of Varnish Films Low-Temperature Coalescence of Latex Paint Films No-Pick-Up Time of Traffic Paint Zinc-Rich Ethyl-Silicate Primers, Resistance to Rubbing with MEK Solvent Cure Times of Ultraviolet-Cured Coatings, Reporting Infi-ared Determination of the Temperature of Applied Coatings on Wood Products During the Curing Cycle Overbaking, Determining Effect on Organic Coatings DRY FILM PROPERTIES Thickness Destructive Measurement of Dry Film Thickness of Protective Coating Systems Measurement of Dry Film Thickness on Ferrous Base Measurement of Dry Film Thickness on Nonfemms Metal Base Micrometer Measurement of Dry-Film Thickness of Organic Coatings Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel Porosity and Permeability Determination of Edge Performance of Composite Wood Products Under Surfactant Accelerated Moisture Stress Porosity of Paint Films Water Vapor Permeability of Organic Coating Films Water Vapor Transmission ofMaterials in Sheet Form (see Vols 04.06, 08.03, and 15.09) Discontinuity (Holiday) Testing of Nonconductive Protective Coating on Metallic Substrates Appearance Properties Gloss, Reflectance, and Hiding Power 45-deg 0-deg, Directional Reflectance Factor of Opaque Specimens by Broad-Band Filter Reflectometry Gloss or Sheen Uniformity, Evaluation of Gloss Differences Between Surfaces of Similar Appearance, Visual Evaluation of Gloss of High-Gloss Surfaces Using Abridged Goniophotpmetry Gloss, Specular Hiding Power of Architectural Paints Applied by Roller Hiding Power of Paints by Reflectometry Hiding Power, Relative, of Paints by the Visual Evaluation of Brushouts Print Resistance of Architectural Paints Reflection Haze of High-Gloss Surfaces Wet-to-Dry Hiding Change Absolute Calibration ofReflectance Standards (see Vol 14.02) Preparation of Reference White Reflectance Standards Selecting Coating Specimens for Appearance Measurements Color Bleeding, Degree of Traffic Paint, Laboratory Determination of '" Color Differences, Calculation frdm Instrumentally Measured Color Coordinates Color Permanence of White Architectural Enamels (Discontinued 1992f) xxvii DUP050297179 Test Methodsfor: D 4960-89 Practicefor: D 3964 - 80 (1989) Test Methodsfor: D 658-91 D 968-81 (1991)" D 4060 - 90 D5181 -91 D 4213 -87 , 03359-90 D2I97 -- 86 (1991)el D 5179-91 D454I -85(1989)" G 10-83(1988) 0 2793 - 69(1987) D 4946 - 89" D 4796 - 88 D3170 - 87 (1991)" D 1642 - 70(1987) D 522-88" D 5178 -91 04145-83 0 3281-84(1989) 04146 - 83(1989)" D 3363-74 (1989)" D 1474-8S (1991)" D 4366 - 91 G 14-88 G 13-89 G 17-88 D 3003-71 (1987) D 2091 -88 D 2794 -90 D 4518-91 D 2370-82 (1987)" D 913-88 Test Methodsfor: 0 3260-82(1991) 0 4938 - 89 D 3623-78a (1987) G 8-90 G 42-90 D 1540 - 82 (1987)" D 1308-87 G 20-88 D 2933-74 (1986)" D 1654-79a (1984)" D 4256-89 D 3719-87 G 19-88 0 2803 - 82(1987) 0 1360 - 90a 0 3806 - 90a D 2485-91 D 3459-87 D 2246 - 87 G 18-88 D 4303-91 D 3424 - 75 D 2620 - 87 D 4939-89 LIST BY SUBJECTS, VOLUME 0KO1 Colot for Thermoplastic Traffic Marking Materials, Evaluation of Selecting of Coating Specimens for Appearance Measurements Physical Strengths and Resistances (Nonchemical) Abrasion Resistance of Organic Coatings by Air-Blast Abrasive Abrasion Resistance of Organic Coatings by Falling Abrasive Abrasion Resistance of Organic Coatings by the Taber Abrasive Abrasion Resistance of Printed Matter by die GA-CAT Comprehensive Abrasion Abrasion Resistance, Wet, of Interior Paints Adhesion by Tape Test, Measuring Adhesion of Organic Coatings by Scrape Adhesion Adhesion of Organic Coatings to Plastic Substrates by Direct Tensile Testing Adhesion Pull-Off Strength of Coatings Using Portable Testers Bendability of Pipeline CoatingsBlock Resistance of Organic Coatings on Wood Substrates Blocking Resistance of Architectural Paints' Bond Strength Test for Thermoplastic Traffic Marking Materials Chipping Resistance of Coatings Elasticity or Toughness of Varnishes Mandrel Bend Test of Coatings, Mar Resistance of Organic Coatings Flexibility, Coating, of Prepainted Sheet Formability of Attached Organic Coatings .with Impact-Wedge Bend Apparatus Formability of Zinc Rich Primer/Chromate Complex Coatings on Steel Hardness, Film, by Pencil Test Hardness, Indentation, of Organic Coatings Hardness Testing of Organic Coatings by Pendulum Damping Impact Resistance of Pipeline Coatings (Failing Weight Test) Impact Resistance of Pipeline Coatings (Limestone Drop Test) Penetration Resistance of Pipeline Coatings (Blunt Rod Test) - ~ Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates Print Resistance of Lacquers Rapid Deformation (Impact), Resistance of Organic Coatings to the Effects of Static Friction of Coating Surfaces, Measuring Tensile Properties of Organic Coatings Wear Resistance of Traffic Paint, Evaluating Degree of Resistances to Chemicals and Environment Acid and Mortar Resistance of Factory-Applied Clear Coatings on Extruded Aluminum Products Antifouling Paints, Erosion Testing, Using High Velocity Water Antifouling Panels in Shallow Submergence, Testing Cathodic Disbdhding of Pipeline Coatings Cathodic Disbonding of Pipeline Coatings Subjected to Elevated Temperatures Chemical Agents, Effect on Organic Finishes tJSed in the Transportation Industry Chemicals, Household, Effect of, oh Gear and Pigmented Organic Finishes Chemical Resistance of Pipeline Coatings I. Corrosion Resistance, Dynamically Testing'Coated Steel Specimens (Discontinued I992f) Corrosive Environments, Evaluation of Painted or Coated Specimens Subjected to Decontaminability of Coatings Used in Light-Water Nuclear Power Plants . Dirt Collection on Exterior White Coated Panels Disbonding Characteristics of Pipeline Coatiiigs by Direct Soil jJurial Filiform Corrosion Resistance of Organic Coatings on Metal ) Fire Retardancy of Paints (Cabinet Method) Fire Retardant Paints, Small Scale Evaluation (2-Foot Tunnel Method) High Temperature Service, Evaluating Coatings Humid-Dry Cycling for Coatings on Wood and Wood Products ' Humidity-Thermal Cycle Cracking, Testing Finishes on Primed Metallic Substrates Joints, Fittings, and Patches in Coated Pipelines Lightfastness of Pigments Used in Artists' Paints Lightfastness of Printed Matter Light Stability of Clear Coatings , Marine Antifouling Coating Subjected to Biofouling and Fljiid Shear Forces in Natural Seawater xxviii Test Methodsfor: D 3274 - 82 (1988)*1 D 3273-86(1991)" D 5108-90 D4828-91 D 4082 -89 B 117-90 D 2486-89 D 2134-66 (1980)" D 2792 - 69 (1987) D2198-84(1989)" D 1211-87 D 3450 -90 D 1647 - 89 G 9-87 E 84-90 E 162-90 Practices for: D 2248 - 89 0 3456 - 86(1991)" D 3023 - 88 D 4585-87" D 870 - 87 D 2247 - 87 D 1735-87 Test Methodsfor: D 868 - 85(1989)" D 714-87 D 659-86" D 660 - 87 |D 661-86" D 662-86" D 772 - 86" D 2200 - 85 (1989) D 610-85(1989)" Practicefor: D4121 - 82 (1987) Test Methodsfor: D 2830 - 91 D 1641-59 (1987) D 1014 - 83 (1988)" D1150-55 (1987)" G 11-88 D 1848-88 Practices for: D4141- 82(1987)" D4587-91 |D 1006 - 73 (1986)" G 23 - 90 D 822 - 89 G 53-88 D 3361-87 D 5031 -90 LIST BY SUBJECTS, VOLUME 06.01 Microbial Growth or Soil and Dirt Accumulation, Evaluating Degree of Surface Disfigurement of Paint Films Mold Growth on the Surface ofInterior Coatings in an Environmental Chamber, Resistance to Oiganotin Release Rates of Antifouling Coating Systems in Sea Water Practical Washability of Organic Coatings Radiation, Effect on Coatings Used in Light-Water Nuclear Power Plants sit Spray (Fog) Testing Scrub Resistance of Interior Latex Flat Wall Paints Softening of Organic Coatings by Plastic Compositions (Discontinued 1990t) Solvent and Fuel Resistance of Traffic Paint Stain Removal from Multicolor Lacquers Temperature-Change Resistance of Clear Nitrocellulose Lacquer Films Applied to Wood Washability Properties of Interior Architectural Coatings Water and Alkali Resistance of Dried Filins of Varnishes Water Penetration into Pipeline Coatings Surface Burning Characteristics ofBuilding Materials (see Vol 04.07) Surface Flammability ofMaterials Using a Radiant Heat Energy Source (see Vol 04.07) Detergent Resistance of Organic'Finishes Microbiological Attack, Determining Susceptibility Of Faint Films by Exterior Exposure Stains and Reagents, Resistance of Factory-Applied Coatings on Wood Products, Determination of Water Resistance of Coatings, Testing Using Controlled Condensation Water Resistance of Coatings, Testing Using.Immersion Water Resistance of Coatings, Testing Using .100 % Relative Humidity Water Resistance of Coatings, Testing Using Water Fog Apparatus Durability Tests Photographic Standards Bleeding of Traffic Paint, Evaluating Degree of Blistering of Paints, Evaluating Degree of' Chalking of Exterior Paints, Evaluating Degree of (Discontinued 1990f--Replaced by Test Methods D4214) Checking of Exterior Paints, Evaluating Degree of Cracking of Exterior Paints, Evaluating Degree of Erosion of Exterior Paints, Evaluating Degree of Flaking (Scaling) of Exterior Paints, Evaluating Degree of Pictorial Surface Preparation Standards for Painting Steel Surfaces . Rusting on Painted Steel Surfaces, Evaluating Degree of Photographic Documentation of Coating and Lining Failures and Defects General Tests Durability and Compatibility of Factory-Primed Wood Products, with Representative Finish Coats Durability of Varnishes, Exterior Exposure Tests of Paints on Steel, Conducting Exterior Exposure Tests of Paints: Single- and Multi-Panel Forms for Recording Results Outdoor Weathering on Pipeline Coatings, Effeetsof Paint Film Failures Characteristic of Exterior Latex Paints, Reporting Exposure Tests of Coatings, Accelerated Outdoor Exposure Tests of Paint and Related Coatings, Conducting Using Fluorescent UV-Condensation Light and Water Apparatus . Exposure Tests of Paints on Wood, Conducting Exterior Light-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Exposure of Nonmetallic Materials, Operating * .- Light- and Water-Exposure Apparatus, Filtered Open-Flame Carbon-Arc Type, for Testing Paint and Related Coatings and Materials Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for Exposure of Nonmetallic Materials, Operating - Light- and Water-Exposure Apparatus (Unfiltered Open-Flame Carbon-Arc Type) for Testing Paint, Varnish, Lacquer, and Related Products Using the Dew Cycle, Operating light- and Water-Exposure, Using Enclosed CarbomArc Apparatus, Conducting Tests on Paints and Related Coatings and Materials xxix DUP050297181 2. LIST:BY SUBJECTS, VOLUME 06.01 Practices for: G 26-90 D 713-90 Test Methods for: D1736-89 D2338 - 84(1989)" D2199-82(1987) D 4797-88 Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of NonmetailicMaterials, Operating Road Service Tests on Traffic Marking Materials, Conducting Miscellaneous Properties Efflorescence of Interior Wall Paints Particle Size of Multicolor Lacquers . Plasticizer Migration from Vinyl Fabrics to Lacquers Thermoplastic Marking, White and Yellow, Containing Lead Chromate and Titanium Dioxide, Chemical Gravimetric Analysis of SCHEDULES OF EXAMINATION FOR TESTING PAINT PRODUCTS Test Methods for: D 1546 - 62 (1987) D 333-87 D 466 - 42(1989) D 2066-91 Practicesfor: D 3794 - 79" D 3002 - 81 (1987) D 3925-81 (1985)" D 3451-76 (1987)" D 3322-82 (1991) D 2336-87 (1991)" Guidesfor: D2833- 89 D 3630 - 89 D3129- 91 D2932- 80 (1988)" D 3730 - 78 (1988)" D4712- 87a (1991) D4540- 91 D 3323 - 80(1988)" D2931- 84 (1989)" D5010- 91 D5146- 91 D 3425 - 80 (1988)" D 3383 - 79a (1988)" D2205- 85 (1990)" D 154- 85(1989)" D 3358 - 88 D2571- 88 Floor Sealers, Clear, Performance Tests of Lacquers; Clear and Pigmented Films Depositedfrom Bituminous Emulsions (see Vol 04.04) Relative Tinting Strength of Printing Ink Dispersions Coil Coatings, Testing Evaluation Of Coatings for Plastids Liquid Paints and Related Pigmented Coatings, Sampling Polymeric Powders and Powder Coatings, Testing Primers and Primer Surfacers Over Preformed Metal, Testing Specifying Properties from Liquid Through. Cured State for Coatings Factory Applied to Wood Products Architectural Paints and Coatings, Index of Methods for Testing Constituents Classified as Hazardous Contained in Protective Coatings Exterior Latex House Paints, Testing Exterior Soivpat-Redneible House and Trim Coatings, Testing High-Performance Interior Architectural Wall Coatings, Testing Industrial Water-Reducible Coatings, Testing Interior Latex Semigloss and Gloss Paints, Testing Interior Solvent-Reducible Flat Wall Paints, Testing Latex Flat Wall Paints, Testing. Printing Inks and Related, Materials, Testing Solvent-Borne Architectural Coatings Solvent-Reducible Interior Semigloss Wall and Trim Enamels, Testing Solvent-Reducible Floor Paints, Testing Traffic Paints, Testing ...... Varnishes, Testing Water-Borne Floor Paints, Testing Wood Furniture Lacquers, Testing Purchasing and Application of Paint and Related Coatings Guidesfor: D 3276 - 86 D 3927 - 87 Painting Inspectors (Metal Substrates)' > State and Institutional Purchasing of Paint* (Intent to Withdraw) > PROTECTIVE COATING AND LINING WORK*'FOR POWER GENERATION FACILITIES Specificationsfor: D 4618-87 D 5139-90 Test Methods for: D 3912-80(1989) D3911 -89 D 4256-89 D4138-88 D4263 - 83 (1988)" D 4285 - 83 (1988) D 4262- 83 (1988) D 4082 - 89 Flue Gas Desulfurization System Components for Protective lining Application Sample Preparation for Qualification Testing of Coatmgsto be Used in Nuclear Power Plants Chemical Resistance of Coatings Used in light-Water Nuclear Power Plants Coatings Used in Light-Water Nuclear Power Plants, Evaluating Decontaminabflity of Coatings Used in Light-Water Nuclear Power Plants, Determination of Dry Film Thickness of Protective Coating Systems by Destructive Means, Measurement of Moisture in Concrete by the Plastic Sheet Method Oil or Water in Compressed Air. pH of Chemically Cleaned orEtched Concrete Surfaces Radiation on Coatings Used in Light-Water Nuclear Power Plants, Effects of f Pr G r S' T P XXX DUPQ50297182 LIST BY SUBJECTS, VOLUME 06.01 - Practices for: D 4259 - 88 D 4260-88 D 4787-88 D 4286-90 D 4227-83 (1989) D 4228 - 83 (1989) D4619-91 D 4121-82 (1987) D 3843-89 D 4257-87 D 4258 - 83 (1988) D4261 - 83 (1988) Abrading Concrete Acid Etching Concrete Continuity Verification of Liquid or Sheet Linings Applied to Concrete Substrates Contractor Qualifications for Nuclear Powered Electric Generation Facilities, Determining Journeyman Painters, Qualification for Application of Coatings to Concrete Surfaces of Safety-Related Areas in Nuclear Facilities Journeyman Painters, Qualification for Application of Coatings to Steel Surfaces of Safety-Related Areas in Nuclear Facilities Linings in Operating Flue Gas Desulfurization Systems, Inspection of Photographic Documentation of Coating and Lining Failures and Defects Quality Assurance for Protective Coatings Applied to Nuclear Facilities Safety Alert Systems for Hazardous Work Locations in the Coatings and Lining Industry (Discontinued 1990+) Surface Cleaning Concrete for Coating Surface Cleaning Concrete Unit Masonry for Coating Guidesfor: D 5161 -91 D 3842 - 86 (1991) D 4537 - 91 D5163-91 Coating and Lining Work (Metal Substrates), Specifying Inspection Requirements for Coatings for Use in Light-Water Nuclear Power Plants, Selection of Test Methods for Qualify and Certify Inspection Personnel for Coating Work in Nuclear Facilities, Establishing Procedures to Safety Related Coatings in an Operating Nuclear Power Plant, Establishing Procedures to Monitor the Performance of Terminology Relating to: D 4538 - 90a Protective Coating and Lining Work for Power Generation Facilities GENERAL STANDARDS Specificationsfor D 3924-80 (1991)<l E 171-87 Standard Environment for Conditioning and Testing Paint Varnish, Lacquer, and Related Materials Standard Atmospheresfor Conditioning and Testing Materials (see Vol 15.09) Test Methodsfor: D 5043 - 90 D 5009-89 D 5066-91 D 95-83(1990) E 306-71 (1976)fl E 337 - 84(1990) Field Identification of Coatings Transfer Efficiency Under Laboratory Conditions, Evaluating and Comparing Transfer Efficiency Under Production Conditions for Spray Application of Automotive Paints--Weight Basis, Determination of Water in Petroleum Products and Bituminous Materials by Distillation Absolute Calibration ofReflectance Standards (see Vol 14.02) Relative Humidity by Wet- and Dry-Bulb Psychrometer (see Vols 07.01,11.03, and 15.09) Practicesfor: D 5064 - 90 D 3980 - 88 D 4236 - 91 D 5068-90 D 5069-90 E 312 - 80(1986) E 179-90 E 167-77(1987) G 24-87 Conducting a Patch Test to Assess Coating Compatibility Interlaboratory Testing of Paint and Related Materials Labeling Art Materials for Chronic Health Hazards Paint Brushes for Evaluation, Preparation of Paint Roller Covers for Evaluation, Preparation of Description and Selection ofConditionsfor Photographing Specimens (see Vol 14.02) Geometric Conditions, Selection of, for Measurement ofReflectance and Transmittance (see Vol 14.02) Goniophotometry ofObjects and Materials (see Vol 14.02) Natural Light Exposure Tests (Sunlight and Daylight), Conducting Under Glass (see Vols 07.01 and 14.02) Definitions ofTerms Relating to: E 284 - 90 E 41-86 D 16-91 Appearance ofMaterials (see Vol 14.02) Conditioning (see Vols 08.03 and 14.02) Paint, Varnish, Lacquer, and Related Products Guides for: D 5065 - 90 D 5063 - 90 Assessing the Condition of Aged Coatings on Steel Surfaces Use of Certification of Coating Conformance Form METRIC PRACTICE Practice for: E 380-91 Use of the International System of Units (SI) (the Modernized Metric System) (Excerpts) (see Related Material section) I xxxi DUP050297183 Designation: B 117 - 90 Standard Test Method of Salt Spray (Fog) Testing1 2 This standard is issued under the fixed designation B 117; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies of the Department ofDefense to replace Method 811.1 ofFederal Test Method Standard No. ISlb. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue that has been adopted by the Department ofDefense. 1. Scope 1.1 This test method sets forth the conditions required in salt spray (fog) testing for specification purposes. Suitable apparatus which may be used to obtain these conditions is described in Appendix XI. The method does not prescribe the type oftest specimen or exposure periods to be used for a specific product, nor the interpretation to be given to tbe results. It should be noted that there is seldom a direct relation between salt spray (fog) resistance and resistance to corrosion in other media, because the chemistry of the reactions, including the formation of films and their protec tive value, frequently varies greatly with the precise condi tions encountered. Comments on the use of the test in research will be found in Appendix X2. For evaluation of corrosive conditions, see Appendix X3. NNO' 1--This method is applicable to salt spray (fog) testing' of ferrous and nonferrous metals, and is also used to test inorganic and organic coatings, etc., especially where such tests are the basis formaterial or product specifications. 1.2 The values stated in SI units are to be regarded as standard. The inch-pound units in parentheses are provided for information. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport toaddress all ofthe safetyproblems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents , 2.1 ASTM Standards: B 287 Method of Acetic Add-Salt Spray (Fog) Testing1 B 368 Method for Copper-Accelerated Acetic Acid-Salt' Spray (Fog) Testing (CASS Test)3 ' 1 This test method is under tbe jurisdiction of ASTM Committee G-l on. Corrosion of Metals, and is the direct responsibility of Subcommittee G01.05 on Laboratory Corrosion Tests. Current edition approved March 30, 1990. Published May 1990. Originally published as B117 - 39 T. Last previous edition B 117 - 85". 2 Discontinued--See 1987 Annual Book ofASTM Standards, Vols 02.05 and 03.02. - .......... ............................... - 3 Annual Book ofASTM Standards. Vol 02.05. '' D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer,, and Related Products4 D1193 Specification for Reagent Water3 D1654 Method for Evaluation of Painted or Coated Spedmens Subjected to Corrosive Environments4 E 70 Test Method for pH of Aqueous Solutions with the Class Electrode6 3. Apparatus 3.1 The apparatus required for salt spray (fog) testing consists of a fog chamber, a salt solution reservoir, a supply of suitably conditioned compressed air, one or more atom izing nozzles, specimen supports, provision for heating the chamber, and necessary means of control. The size and detailed construction ofthe apparatus are optional, provided the conditions obtained meet the requirements of this method. 3.2 Drops of solution which accumulate on the ceiling or cover of the chamber shall not be permitted to fall on the spedmens being tested. 3.3 Drops of solution which fall from the spedmens shall not be returned to the solution reservoir for respraying. 3.4 Material of construction shall be such that it will not affect the corrosiveness of the fog. 4. Test Specimens 4.1 The type and number of test specimens to be used, as well as the criteria for the evaluation ofthe test results, shall be defined in the specifications covering the material or product being tested or shall be mutually 'agreed upon by the purchaser and the seller. 5. Preparation of Test Specimens , 5.1 Metallic and metallic-coated specimens shall be suit ably cleaned. The cleaning method shall be optional de pending on the nature of the surface and file contaminants, except that it shall not include the use ofabrasives other than a paste of pure magnesium oxide nor of solvents which are corrosive or will deposit either corrosive or protective films. The use of a nitric add solution for the chemical cleaning, or passivation, of stainless steel spedmens is permissible when agreed upon by the purchaser and the seller. Care shall be taken that specimens are not recontaminated after cleaning by excessive or. careless handling. * Annual Book ofASTM Standards, Vol 06-01. 5 Annual Book ofASTM Standards, Vol 11.01. 4 Annual'Book ofASTM Standards, Vol 15.05. DUP050297184 B 117 5.2 Specimens for evaluation of paints and other organic Ratings shall be prepared in accordance with applicable gpecification(s) for the materials) being tested, or as agreed upon by the purchaser and supplier. Otherwise, the test specimens shall consist of steel meeting the requirements of Methods D609 and shall be cleaned and prepared for coating in accordance with applicable procedure of Methods D 609. 5.3 Specimens coated with paints or nonmetallic coatings shall not be cleaned or handled excessively prior to test. 5.4 Whenever it is desired to determine the development of corrosion from an abraded area in the paint or organic coating, a scratch or scribed line shall be made through the coating with a sharp instrument so as to expose the under lying metal before testing. The conditions of making the scratch shall be as defined in Method D 1654, unless otherwise agreed upon between the purchaser and seller. 5.5 Unless otherwise specified, the cut edges of plated, coated, or duplex materials and areas containing identifica tion marks or in contact with the racks or supports shall be protected with a suitable coating stable under the conditions of the test, such as ceresin wax. NPQ' 2--Should it be desirable to cut test specimens from parts or from preplated, painted, or otherwise coated steel sheet, the cut edges shall be protected by coating them with paint, wax, tape, or other, effective media so that the development of a galvanic effect between such edges and the adjacent plated or otherwise coated metal surfaces, is prevented. 6. Position of Specimens During Test 6.1 The position of the specimens in the salt spray chamber during the test shall be such that the following conditions are met 6.1.1 Unless otherwise specified, the specimens shall be supported or suspended between 15 and 30 from the vertical and preferably parallel to the principal direction of hori zontal flow of fog through the chamber, based upon the dominant surface being tested. 6.1.2 The specimens shall not contact each other or any metallic material or any material capable of acting as a wick. 6.1.3 Each specimen shall be so placed as to permit free settling of fog on all specimens. 6.1.4 Salt solution from one specimen shall not drip on any other specimen. NRS' 3--Suitable materials for the construction or coating of racks and supports are glass, rubber, plastic, or suitably coated wood. Bare metal shall not be used. Specimens shall preferably be supported from the bottom or the side. Slotted wooden strips are suitable for the support offlat panels. Suspension from glass hooks or waxed string may be used as long as the specified position ofthe specimens is obtained, ifnecessary by means of secondary support at the bottom of the specimens. 7. Salt Solution 7.1 The salt solution shall be prepared by dissolving 5 1 parts by weight of sodium chloride in 95 parts of water conforming to Type IV water in Specification D 1193. The salt used shall be sodium chloride substantially free of nickel and copper and containing on the dry basis not more than 0.1 % of sodium iodide and not more than 0.3 % of total impurities. Some salts contain additives that may act as corrosion inhibitors; careful attention should be given to the chemical content of the salt. Upon agreement between purchaser and seller, analysis may be required and limits established for elements or compounds not ^^ chemical composition given above. 7.2 The pH of the salt solution shall be such that when atomized at 35C (95F) the collected solution will be in the pH range of 6.5 to 7.2 (Note 4). Before the solution is atomized it shall be free of suspended solids (Note 5). The pH measurement shall be made electrometrically at 25C (77F) using a glass electrode with a saturated potassium chloride bridge in accordance with Method E70, or colorimetrically using bromothymol blue as indicator, or short range pH paper which reads in 0.2 or 0.3 of a pH unit (Note 6). NTU' 4--Temperature affects the pH of a salt solution prepared from water saturated with carbon dioxide at room temperature and pH adjustment may be made by the following three methods: (f) When the pH of a salt solution is adjusted at room temperature and atomized at 35C (95F), the pH of the collected solution will be higher than the original solution due to the loss ofcarbon dioxide at the highertemperature. When the pH ofthe salt solution is adjusted at room temperature, it is therefore necessary to adjust it below 6.5 so the collected solution after atomizing at 35*C (95'F) will meet the pH limits of6.5 to 7.2. Take about a 50-mL sample ofthe salt solution as prepared at room temperature, boil gently for 30 s, cool, and determine the pH. When the pH of the salt solution is adjusted to 6.5 to 7.2 by this procedure, the pH ofthe atomized and collected solution at 35"C (95'F) will come within this range. (2) Heating the salt solution to boiling and cooling to 95'F for maintaining it at 95'F for approximately 48 h before adjusting the pH produces a solution the pH of which does not materially change when atomized at 35C (95'F). (5) Heating the water from which the salt solution is prepared to 35'C (95"F) or above, to expel catbon dioxide, and adjusting the pH of the salt solution within the limits of 6.5 to 7.2 produces a solution the pH of which does not materially change when atomized at 35'C (95'F). NVW' 5--The freshly prepared salt solution may be filtered or decanted before it is placed in the reservoir, or the end of the tube leading from the solution to the atomizer may be covered with a double layer of cheesecloth to prevent plugging of the nozzle. NVW' 6--The pH can be adjusted by additions of dilute cp hydro chloric acid or cp sodium hydroxide solutions. 8. Air Supply 8.1 The compressed air supply to the nozzle or nozzles few atomizing the salt solution shall be free of oil and dirt (Note 7) and maintained between 69 and 172 kN/m2 (10 and 25 psi) (Note 8). NTU' 7--The air supply may be freed from oil and dirt by passing it trough a water scrubber or at.legst 610 mm (2 ft) of suitable cleaning laterial such as sheep's wool, excelsior, slag wool, or activated iuNmViWn'a.S--Atomizing nozzles may have a "critical pressure" at which n abnormal increase in the corrosiveness of the salt fog occurs. If the :ritical pressure" of a nozzle has not been established with certainty jntrol of fluctuation in the air pressure within plus orminus 0.7 kN/nr ).l psi), by installation of a suitable pressure regulator valve mint- 1 Registered U. S. Patent Office. ., !The Nullmatic pressure regulator (or equivalent) manufactured oy MW> ducts Co., H and Lycoming Sts, Philadelphia, PA 19124, a suitable for dm 2 I mizes pressr 9. O 9.1 ' chare 3F). cabin (exce spray renao soluti Noi contin from i obtain< becaus 9.2 fog co no dr i source ; proxit , and tf that ft be col per he The sc shall t solutic made thymo Non inserted dishes, about 8' Non 25'C (T may ala to 100 aliquot water ai titrate v perman raL of requirer 9.3 that ni specimi 10. Coi 10.1 ering tk continu uous op spray c (0.J DUP050297185 B 117 mizes the possibility that the nozzle will be operated at its "critical pressure."9 9. Conditions in the Salt Spray Chamber 9.1 Temperature--The exposure zone of the salt spray chamber shall be maintained, at 35 + 1.1 - 1.7'C (95 + 2 -- 3'F). The temperature within the exposure zone ofthe closed cabinet shall be recorded at least twice a day at least 7 h apart (except on Saturdays, Sundays, and holidays when the salt spray test is not interrupted for exposing, rearranging, or removing test specimens or to check and replenish the solution in the reservoir). NXY' 9--A suitable method to record the temperature is by a continuous recoiding device or by a thermometer which can be read from outside the closed cabinet. The recorded temperature must be obtained with the salt spray chamber to avoid a false low reading because of wet-bulb effect when the chamber is open. 9.2 Atomization and Quantity ofFog--At least two clean fog collectors shall be so placed within the exposure zone that no drops of solution from the test specimens or any other source shall be collected. The collectors shall be placed in the proximity of the test specimens, one nearest to any nozzle and the other farthest from all nozzles. The fog shall be such that for each 80 cm2 of horizontal collecting area there will be collected in each collector from 1.0 to 2.0 mL of solution per hour based on an average run of at least 16 h (Note 10). The sodium chloride concentration of the collected solution shall be 5 1 weight % (Note 11). The pH of the collected solution shall be 6.5 to 7.2. The pH measurement shall be made electrometrically or colorimetrically using bromothymol blue as the indicator. NZ[' 10--Suitable collecting devices are glass funnels with the stems inserted through stoppers into graduated cylinders, or crystallizing dishes. Funnels and dishes with a diameter of 10 cm have an area of about 80 cm2. NXY' 11--A solution having a specific gravity of 1.0255 to 1.0400 at 25C (77"F) will meet the concentration requirement. The concentration may also be determined as follows: Dilute 5 mL ofthe collected solution to 100 mL with distilled water and mix thoroughly; pipet a 10-mL aliquot into an evaporating dish or casserole; add 40 mL of distilled water and 1 mL of 1 % potassium chromate solution (chloride-free) and titrate with 0.1 N silver nitrate solution to the first appearance of a permanent red coloration. A solution that requires between 3.4 and 5.1 mL of 0.1 N silver nitrate solution will meet the concentration requirements. 9.3 The nozzle or nozzles shall be so directed or baffled that none of the spray can impinge directly on the test specimens. 10. Continuity of Test 10.1 Unless otherwise specified in the specifications cov ering the material or product being tested, the test shall be continuous for the duration ofthe entire test period. Contin uous operation implies that the chamber be closed and the spray operating continuously except for the short daily 9 It has been observed that periodic fluctuations in air pressure of 3.4 kN/m2 (0.5 psi) resulted in about a twofold increase in the corrosivity of the fog from a nozzle which was being operated at an average pressure of 110 kN/m2 (16 psi). Controlling the fluctuations within 0.7 kN/m2 (0.1 psi). however, avoided any increase in the corrosivity of the salt fog. See Darsey, V. M. and Cavanagh, W. R., "Apparatus and Factors in Salt Fog Testing," Proceedings, ASTM, Vol 48, 1948, p. 153. interruptions necessary to inspect, rearrange, or remove test specimens, to check and replenish the solution in the reservoir, and to make necessary recordings as described in Section 9. Operations shall be so scheduled that these interruptions are held to a minimum. 11. Period of Test 11.1 The period of test shall be as designated by the specifications covering the material or product being tested or as mutually agreed upon between the purchaser and the seller. NZ[' 12--Recommended exposure periods are to be as agreed upon by the purchaser and seller, but exposure periods of multiples of24 h are suggested. 12. Oeaning of Tested Specimens 12.1 Unless otherwise specified in the specifications cov ering the material or product being tested, specimens shall be treated as follows at the end of the test: 12.1.1 The specimens shall be carefully removed. 12.2 Specimens may be gently washed or dipped in dean running water not warmer than 38C (100'F) to remove salt deposits from their surface, and then immediately dried. Drying shall be accomplished with a stream of dean, compressed air. 13. Evaluation of Results 13.1 A careful and immediate examination shall be made for the extent of corrosion of the dry test specimens or for other failure as required by the specifications covering the material or product being tested or by agreement between the purchaser and the seller. 14. Records and Reports 14.1 The following information shall be recorded, unless otherwise prescribed in the spedfications covering the mate rial or product being tested: 14.1.1 Type of salt and water used in preparing the salt solution, 14.1.2 All readings of temperature within the exposure zone of the chamber, 14.1.3 Daily records of data obtained from each fogcollecting device including the following: 14.1.3.1 Volume of salt solution collected in millimetres per hour per 80 cm2, 14.1.3.2 Concentration or specific gravity at 35C (95F) of solution collected, and 14.1.3.3 pH of collected solution. 14.4 Type of specimen and its dimensions, or number or description of part, 14.5 Method of cleaning spedmens before and after testing, 14.6 Method of supporting or suspending article in the salt spray chamber, 14.7 Description of protection used as required in 5.5, 14.8 Exposure period, 14.9 Interruptions in test, cause and length of time, and 14.10 Results of all inspections. NZ[' 13--If any of the atomized salt solution which has not contacted the test specimens is returned to the reservoir, it is advisable to record the concentration or specific gravity of this solution also. 3 DUP050297186 # B 117 15. Precision and Bias10 15.1 The reproducibility of results in the salt spray test is highly dependent on the type of specimens tested and the evaluation criteria selected as well as the control of the operating variables. In any testing program, sufficient repli cates should be included to establish the variability of the results. Substantial variability is often observed when similar specimens are tested in different fog chambers even, though 10 Supporting data are available on loan from ASTM Headquarters. Request RRrGOt-1003. the testing conditions are nominally similar and within the ranges specified in this method. 15.2 The salt spray (fog) test is intended to reproduce the corrosion that occurs in atmospheres containing salt spray or splash. It has been widely observed, however, that rankings of different alloys or coating systems, or both, do not necessarily fall in the same order as atmospheric tests in marine or road salt splash environments. This test has been more useful in rating the relative resistance of a specific type of protective coating, for example, hot-dip zinc coatings on steel. Interpretation of the results of this method beyond this purpose must be verified by actual exposure tests. APPENDIXES (Nonmandatory Information) XI. CONSTRUCTION OF APPARATUS X1.1 Cabinets XI. 1.1 Standard salt spray cabinets are available from several suppliers, but certain pertinent accessories are re quired before they will function according to this method and provide consistent control for duplication of results. XI. 1.2 The salt spray cabinet consists of the basic chamber, an air-saturator tower, a salt solution reservoir, atomizing nozzles, specimen supports, provisions for heating the chamber, and suitable controls for maintaining the desired temperature. XI. 1.3 Accessories such as a suitable adjustable baffle or central fog tower, automatic level control for the salt reservoir, and automatic level control for the air-saturator tower are pertinent parts of the apparatus. XI. 1.4 The cabinet should be of sufficient size to test adequately the desired number of parts without over crowding. Small cabinets have been found difficult to control Siphon Height, In. 4 8 12 16 TABLE X1.1 Operating Characteristics of Typical Spray Nozzte Air Flow, L/mln Solution Consumption, mL/h Air Pressure, psl Air Pressure, psl S 10 15 20 5 10 . 15 20 19 26.5 31.5 19 26.5 31.5 19 26.5 31.5 19 26.6 31.5 36 36 36 36 '2100 636 0 0 3840 2760. 1380 780- 4584 3720 3000 2124 5256 4320 3710 2904 . Siphon Height cm 10 20 30 40 Air Flow, dm3/mln , ..... ...... --..... ....----------------- Air Pressure, kPa 34 69 103 138 191 26.5 31.5 19 26.5 31.5 19 26.5 31.5 19 26.6 31.5 36 36 36 36 ' Solution Consumption, cm3/h , Air pressure, kPa 34 69 103 138 2100 636 0 0 3840 2760 1380 780 4584 3720 3000 2124 5256 4320 3710 2904 and those of less than 0.43-m3 (15-ft3) capacity should be avoided. X1.1.5 The chamber may be made of inert materials such as plastic, glass, or stone, but most preferably is constructed of metal and lined with impervious plastics, rubber, or epoxy-type materials or equivalent. XI .2 Temperature Control XI.2.1 The maintenance of temperature within the salt chamber can be accomplished by several methods. It is generally desirable to control the temperature of the sur roundings of the salt spray chamber and to maintain it as stable as possible. This may be accomplished by placing the apparatus in a constant-temperature room, but may also be achieved by surrounding the basic chamber of a jacket containing water or air at a controlled temperature. X 1.2.2 The use of immersion heaters in an internal salt solution reservoir or of heaters within the chamber is detrimental where heat losses are appreciable, because of solution evaporation and radiant heat on the specimens. Xl.2.3 All piping which contacts the salt solution or spray should be of inert materials such as plastic. Vent piping should be of sufficient size so that a minimum of back pressure exists and should be installed so that no solution is trapped. The exposed end of the vent pipe should be shielded. from extreme air currents that may cause fluctuation of pressure or vacuum in the cabinet XU Spray Nozzles XI .3.1 Satisfactory nozzles may be made of hard rubber, plastic, or other inert materials. The most commonly used type is made of plastic. Nozzles calibrated for air consump. tion and solution-atomized are available. The operating characteristics of a typical nozzle are given in Table XI.1. X 1.3.2 It can readily be seen that air consumption is relatively stable at the pressures normally used, but a marked reduction in solution sprayed occurs if the level' of the solution is allowed to drop appreciably during the test. Thus, DUP050297187 i the e the ay or dugs not ts in been type js on i this Id be such acted r, or } salt It is surit as gthe so be acket 1 salt er is se of of bber, used ump ating l.l. on is arked f the rhus, a--Angle of lid, 90 to 125* 1-- Thermometer and thermostat for controlling heater (Item No. 8) in base 2-- Automatic water levelling device 3-- Humidifying tower 4-- Automatic temperature regulator for controlling heater (Item No. 5) 5-- immersion heater, nonrusting 6-- Air Inlet, multiple openings 7-- Air tube to spray nozzle 8-- Strip heater In base 9-- Hinged top, hydraulically operated, or counterbalanced 10-- Brackets for rods supporting specimens, or test table 11-- Internal reservoir 12-- Spray nozzle above reservoir, suitably designed, located, and baffled 12A--Spray nozzle housed In dispersion tower located preferably In center of cabinet 13-- Water seal 14-- Combination drain and exhaust Exhaust at opposite side of test space (tom spray nozzle (Item 12), but preferably in combination with drain, waste trap, and farced draft waste pipe (items 16,17, and 19). 16-- Complete separation between forced draft waste pipe (Item 17) and combination drain and exhaust (Items 14 and 19) to avoid undesirable suction or back pressure. 17-- Forced draft waste pipe 18-- Automatic levelling device far reservoir 19-- Waste trap 20-- Air space or water jacket 21-- Test table or rack, well below roof area FIG. XI.1 Typical Salt Spray Cabinet the level of the solution in the salt reservoir must be maintained automatically to ensure uniform fog delivery during the test11 X 1.3.3 If the nozzle selected does not atomize the salt solution into uniform droplets, it will be necessary to direct the spray at a baffle or wall to pick up the larger drops and prevent them from impinging on the test specimens. Pending a complete understanding of air-pressure effects, etc., it is important that the nozzle selected shall produce the desired condition when operated at the air pressure selected. Nozzles are not necessarily located at one end, but may be placed in the center and can also be directed vertically up through a suitable tower. XI.4 Air for Atomization X 1.4.1 The air used for atomization must be free of grease, oil, and dirt before use by passing through wellmaintained filters. Room air may be compressed, heated, humidified, and washed in a water-sealed rotary pump, if the temperature of the water is suitably controlled. Otherwise 1' A suitable device for maintaining the level of liquid in either the saturator tower or reservoir oftest solution may be designed by a local engineering group, or may be purchased from manufacturers of test cabinets as an accessory. cleaned air may be introduced into the bottom of a tower filled with water, through a porous stone or multiple nozzles. The level of the water must be maintained automatically to ensure adequate humidification. A chamber operated ac cording to this method and Appendix will have a relative humidity between 95 and 98 %. Since salt solutions from 2 to 6 % will give the same results (though for uniformity the limits are set at 4 to 6 %), it is preferable to saturate the air at temperatures well above the chamber temperature as insur ance of a wet fog. Table X1.2 shows the temperatures, at different pressures, that are required to offset the cooling effect of expansion to atmospheric pressure. X 1.4.2 Experience has shown that most uniform spray chamber atmospheres are obtained by increasing the atom- TABLE X1.2 Temperature and Pressure Requirements (or Operation of Test at 95F Air Pressure, pal 12 14 16 18 Temperature, F 114 117 119 121 Air Pressure, kPa Temperature, C 83 96 110 124 48 47 48 49 DUP050297188 B 117 N\]' --^_' controls are the same, In general as for the laboratory cabinet (Fig. XI .1), but are sized to care for the larger cube. The chamber has the Mowing features: (f) Heavy Insulation, (2) Refrigeration door with drip rail, or pressure door with drip rail, inwardsloping sill, (3) Low-temperature auxiliary heater, and (4) Duck boards on floor, with floor sloped to combination drain and air exhaust. FIG. X1.2 Walk-in Chamber, 1.5 by 2.4 m (5 by 8 ft) and Upward fn Overall Size izing air temperature sufficiently to offset heat losses, except those that can be replaced otherwise at very low-temperature gradients. XI3 Types of Construction X 1.5.1 A modem laboratory cabinet is shown in Fig. Xl.l. Walk-in chambers are not usually constructed with a sloping ceiling due to their size and location. Suitably located and directed spray nozzles avoid ceiling accumulation and drip. Nozzles may be located at the ceiling, or 0.91 m (3 ft) from the floor directed upward at 30 to 60' over a pas sageway. The number of nozzles depends on type and capacity and is related to the area of the test space. An 11- to 19-dm3 (3- to 5-gal) reservoir is required within the chamber; with the level controlled. The major features of a walk-in type cabinet, which differs,significantly from the laboratory type, are illustrated in Fig; XI.2. Construction of a plastic nozzle, such as is furnished by several suppliers, is shown in Fig. XI.3. ' I X3. | proc salt si steel t a spec more is also differe X3. 127 nr grade X3. | before i of dirt I test re f balanc X3. two w suppo X2. USE OF THE SALT SPRAY (FOG) TEST IN RESEARCH X2.1 The detailed requirements of this method are pri marily for quality acceptance and should not be construed as([ the optimum conditions for research studies. The test has been used to a considerable extent for the purpose of comparing different materials or finishes with an acceptable standard. The recent elimination of many cabinet variablesand the improvement in controls- have made the three ASTM Salt Spray Tests: Method B 117, B 287, and B 368, into useful tools for many industrial and military production and qualification programs. X2.2 The test has been used to a considerable extent for the purpose of comparing different materials or finishes. It should be noted that there is seldom a direct relation between salt spray (fog) resistance and resistance to corrosion in other media, because the chemistry of the reactions/ including the formation of films and their protective value, frequently varies greatly with the precise conditions encoun tered. Informed personnel are'aware of the erratic composi tion of basic alloys, the possibility of wide variations in quality and thickness of plated items produced on the same racks at the same time, and the consequent need for a mathematical determination of the number of specimens required to constitute an adequate sample for test purposes, In this connection it is well to point out that Method B M 7 is not applicable to the study or testing ofdecorative chromium plate (nickel-chromium or copper-nickel-chromium) on steel or on zinc-base die castings or ofcadmium plate on steel. For this purpose Methods B 287 and B 368 are available, which are iso considered by some to be superior for comparison of chemically-treated aluminum (chromated, phosphated, or anodized), although final conclusions regarding the validity of test results related to service experience have not been reached. Method B 117 is considered to be most useful in estimating the relative behavior ofclosely related materials in marine atmospheres, since it simulates the basic conditions with some acceleration due to either wetness or temperature or both. X2.3- When a test is used for research, it may prove advantageous to operate with a different solution composi tion or concentration or at a different temperature. In all cases, however, it is desirable to control,the temperature and humidity in the manner specified, and to make certain that the composition of the settled fog and that of the solution in the reservoir are substantially the same. Where differences.develop, it is necessary to .control conditions so that .the characteristics of the settled fog meet the specified require ments for the atmosphere. : X2.4 Material specifications should always be written in^ terms of the standard requirements of the appropriate salt spray method, thereby making it possible to test a variety of materials from different sources in the same equipment. ... [ j j ; l j 6 dririiili DUP050297189 E X3. EVALUATION OF CORROSIVE CONDITIONS ia ed ad ft) asnd to er, -in >ry tic in teel For ich lof or lity een 1 in Is in ions ture -ove >osii all and that n in aces the uire- n in salt ty of X3.1 General--This appendix covers test panels and procedures for evaluating the corrosive conditions within a salt spray cabinet The procedure involves the exposure of steel test panels and the determination of their mass losses in a specified period of time. This may be done monthly or ore frequently to insure consistent operation over time. It is also useful for correlating the corrosive conditions among different cabinets. X3.2 Test Panels--The required test panels, 76 mm by 127 nun by 0.8 mm, are made from SAE 1010 commercial grade cold-rolled carbon steel (UNS G10080). X3.3 Preparation ofPanels Before Testing--Clean panels before testing by degreasing only, so that the surfaces are free of dirt, oil, or other foreign matter that could influence the test results. After cleaning, weigh each panel on an analytical balance to the nearest 1.0 mg and record the mass. X3.4 Positioning of Test Panels--Place a minimum of two weighed panels in the cabinet, with the 127-mm length supported 30 from vertical. Place the panels in the prox imity of the condensate collectors. (See Section 6.) X3.5 Duration of Test--Expose panels to the silt fog for 48 to 168 h. X3.6 Cleaning of Test Panels After Exposure--After re moval of the panels from the cabinet, rinse each panel immediately with running tap water to remove salt, and rinse in reagent grade water (see Specification D 1193, Type IV). Chemically clean each panel for 10 min at 20-25C in a fresh solution prepared as follows: Mix 1000 mL of hydrochloric acid (Sp. Gr. 1.19) with 1000 mL reagent grade water (D 1193, Type IV) and add 10 grams of hexamethylene tetramine. After cleaning, rinse each panel with reagent grade water (Type IV) and dry (see 12.2). X3.7 Determining Mass Loss--Immediately after drying, determine the mass loss by reweighing and subtracting panel mass after exposure from its original mass. The mass should not vary 20 % from test to test. X3.7.1 Data generated in the Interlaboratory Study using this method are available from ASTM as Research Report. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race Si, Philadelphia, PA 19103. DUP050297190 Last ASTM Designation: B 287 - 74 (1980f Standard Method of Acetic Acid-Salt Spray (Fog) Testing This method sets forth the conditions required in acetic add-salt spray (fog) testing for spedfication purposes. Formerly under the jurisdiction of Committee G-l on Corrosion of Metals, this method was discontinued in 1988 and replaced by G 85. abrasi resis app< sera] acid m siuir add: gene acid vc acrylic adhesi< adde subs spec: alkyd) archite tion I cial, asbestc type. associa hydr phot visco parti prest than the t autode] cess ! uniq aque. Com tions to dt dispe I DiS' rate o pretret and gi Itregul 1 These paint and Subcommi Current Published; 8 DUP050297191 Designation: D 16 - 91 Standard Terminology Relating to Paint, Varnish, Lacquer, and Related Products1 This standard is issued under the fixed designation D 16; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision, A number in parentheses indicates the year of last reapproval. A supeiscript epsilon () indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by ike Department ofDefense. abrasion resistance (coatings)--the ability of a coating to resist being worn away and to maintain its original appearance and structure when subjected to rubbing, scraping, or wear. acid number (coatings)--the number of milligrams of potas sium hydroxide (KOH) required to neutralize the free acids in 1 g of an oil, resin, varnish, or other substance; generally reported on the nonvolatile content. acid value (coatings)--see add number. acrylic resin--under resin, synthetic, see acrylic resin. adhesion promoters--materials built into the binder or added to the paint to form primary bonds to either the substrate or the previously applied coating with the specific aim ofimproving the dry or wet adhesion, or both. alkyd resin--under resin, synthetic, see alkyd resin. architectural coatings--coatings intended for on-site applica tion to interior or exterior surfaces of residential, commerdal, institutional or industrial buildings. asbestos--see industrial talc and industrial talc, nonasbestos type. associative thickener--water soluble polymers containing hydrophobic groups that are capable of nonspedfic hydrophobic association similar to surfactants that elevate viscosity presumably by assodation between thickener partides or thickener and dispersed particles that may be present in the aqueous system such as latex particles rather than through high molecular weight or chain stiffness of the thickener molecules themselves, autodeposition--a single-step immersion metal finishing pro cess in which an organic coating is applied by means of unique surface chemical reactions carried out in an aqueous latex dispersion, also referred to as chemiphoresis. Components within the bath give rise to chemical reac tions that slightly solubilize the metallic surface and lead to destabilization, deposition, and coalescence of the dispersed latex particles at that surface. `D< ( a``< bn--The deposition rate of the latex is controlled by the rate of surface solubilization. The process does not require any pretreatments such as phosphating, needs no external energy input, and gives rise to deposition wherever the solution wets the substrate. Irregularly shaped parts can be uniformily coated. 1 These definitions are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.16 on Definitions. Current edition approved Oct. 15, 1991. Published December 1991. Originally published as D 16 - 11. Last previous edition D 16 - 90a. baking finish--a paint or varnish that requires baking at temperatures above 150T (65C) for the development of desired properties. baking temperature--a temperature above 150F (65C). batch--the total quantity of a material produced in a single final mixing operation after all production processes are complete, or just prior to filling. bituminous varnish--under varnish, see bituminous varnish. bleeding--the diffusion of coloring matter through a coating from the substrate; also, the discoloration arising from such diffusion. In the case of printing ink, the spreading or running of a pigment color by the action of a solvent such as water or alcohol. blistering resistance (coatings)--the ability of a coating to resist the formation in the film of dome-shaped, liquid- or gas-filled projections resulting from local loss of adhesion and lifting of the film from the previously applied coating or the substrate. bulking value--solid volume of a unit weight of material, usually expressed as gallons per pound. For practical purposes this is 0.120 divided by the specific gravity, caulking compound--a soft, plastic material, consisting of pigment and vehicle, used for sealing joints in buildings and other structures where normal structural movement may occur. Caulking compound retains its plasticity for an extended period after application. It is available in forms suitable for application by gun and knife and in extruded preformed shapes. cellulose lacquer--see lacquer. chalking resistance (coatings)--the ability of a pigmented coating to resist the formation of a friable powder on its surface caused by the disintegration of the binding me dium by degradative weather factors, checking resistance (coatings)--the ability of a coating to resist slight breaks in the film that do not penetrate to the previously applied coating or to the substrate. The breaks should be called cracks if penetration extends to the previously applied coating or to the substrate. See cracking resistance. chipping resistance (coatings)--the ability of a coating or layers ofcoatings to resist removal, usually in small pieces, resulting from impact by hard objects or from wear during service. coating--a liquid, liquefiable or mastic composition that is converted to a solid protective, decorative, or functional adherent film after application as a thin layer, color of an object--the aspect of the appearance of an object dependent upon the spectral composition of the incident light, the spectral reflectance or transmittance of the 9 DUP050297192 D 16 object, and the spectral response of the observer, hue--the attribute by which a perceived color is distin guished as red, yellow, green, blue, purple, or a combina tion of these. (White, gray, and black colors possess no hue.) lightness--the attribute by which a perceived color is judged to be equivalent to a member of the continuous series of grays ranging from black to white. saturation--the attribute by which a perceived color is judged to depart from gray of equal lightness toward a pure hue. contrast ratio--ratio of the reflectance of a dry paint film over a black substrate of 5 % or less reflectance, to the reflectance of the same paint, equivalently applied and dried, over a substrate of 80 % reflectance, coverage, coverage rate, covering power--ambiguous terms that are used in some instances to refer to hiding power and in others to mean spreading rate. The precise terms hiding power and spreading rate are preferred, cracking resistance (coatings)--the ability of a coating to resist breaks of the film where the breaks extend through to the surface painted and the previously applied coating or the substrate is visible. The use of a minimum magnifi cation of 10 diameters is recommended in cases where it is difficult to differentiate between cracking and checking. See checking resistance. dirt (coatings)--see soil. dirt resistance (coatings)--the ability of a coating to resist soiling by foreign material, other than microorganisms, deposited on or embedded in the dried coating, distinctness-of-image gloss--the sharpness with which image outlines are reflected by the surface of an object, dope--a composition, usually a cellulosic lacquer, for appli cation on textiles and leathers, drier--a composition that accelerates the drying of oil, paint, printing ink, or varnish. Driers are usually metallic com positions and are available in both solid and liquid forms, drying oil--an oil that possesses to a marked degree the property of readily taking up oxygen from the air and changing to a relatively hard, tough, elastic substance when exposed in a thin film to the air. durability--a relative term indicating degree of permanency. It may be applied to individual protective, decorative, or functional properties, for example, "the durability of gloss," but if used in a general way, for example, "the excellent durability of a paint," implies the ability of the described coating to retain, to the indicated degree, all the properties required for the continued service of the coating. edge-tracking (coatings)--a residual, discernible pattern in a roller-applied coating characterized by trails from either or both ends of the roller. emulsion paint--under paint, see emulsion paint. enamel--a paint that is characterized by an ability to form an especially smooth film. erosion resistance (coatings)--the ability of a coating to withstand being worn away by chalking or by the abrasive action of water or windbome particles of grit. The degree of resistance is measured by the amount of the coating retained. See abrasion resistance. ester gum--under resin, synthetic, see ester gym. extended pigments--organic pigments diluted with an ex tender (for example, alumina trihydrate, blanc fixe, or calcium carbonate). filler--a pigmented composition for filling the pores or irregularities in a surface preparatory to application of other finishes. fire-retardant--a descriptive term which implies that the described product, under accepted methods of test, will significantly: (a) reduce the rate of flame spread on the surface of a material to which it has been applied, or (M resist ignition when exposed to high temperatures', or (c) insulate a substrate to which it has been applied and prolong the time required to reach its ignition, melting, or structural-weakening temperature, filiform corrosion resistance (coatings)--the ability of a coating to resist that type of corrosion of metal substrates characterized by a definite thread-like structure and direc tional growth that occurs under coatings, fire-retardant coating--a coating that will do one or more of the following: (1) reduce the flame spread on the substrate over which the coating is applied, sometimes at the sacrifice of the coating (see intumescent coating); (2) resist ignition of the substrate when exposed to high tempera ture; or (2) insulate the substrate to which the coating is applied and thereby prolong the time required to reach its ignition, melting or structural-weakening temperature, flaking resistance (coatings)--the ability of a coating to resist the actual detachment of film fragments either from the previously applied coating or the substrate. Flaking is generally preceded by cracking, checking, or blistering and is the result of loss of adhesion. Also known as scaling resistance. flatting agent--a material added to paints, varnishes, and other coating materials to reduce the gloss of the dried film. forced drying temperature--a temperature between room temperature and 150F (65C). fossil resin--under resin, natural, see fossil resin. gallon, U. S.--a volume equal to 231 in.3 For paint, varnish, lacquer, and related products this is measured at 77F (25'C). glaze--a very thin coating of a paint product usually a semi-transparent coating tinted with Van Dyke brown, burnt sienna, or a similar pigment, applied on a previously painted surface to produce a decorative effect, glaring compound--a dough-like material consisting of pig ment and vehicle, used for sealing window glass in frames. It differs from putty in that it retains its plasticity for an extended period. } grindingjapan--see japan, grinding, grit--the coarse foreign particles in paint materials and coatings, often of irregular shape, that are hard, abrasive, and resistant to disintegration. hiding power--the ability of a paint, or paint material as ; used, to hide or obscure a surface to which it has been ; uniformly applied. When expressed numerically, it is . generally in terms of the number ofsquare feet over which j j a gallon of paint, or pound of pigment, as used, can be uniformly spread to produce a specified contrast ratio (see i 10 0. CO re. huehydr hy g< indu: frc M as: de A: as indu les ar be as to re: nc as intui th nc m ca th japa Ja te japa japa ja japa lacq th sc ic Ct lake 0 d 17 P ty by 01 si cc SL PI CC as lap< m C DUP050297193 th an ex; fixe, or pores or cation of that the test, will id on the ed, or (6) res, or (c) plied and lelting, or lity of a substrates ind direc- r more of substrate ;s at the (2) resist tempera coating is > reach its ature. gto resist from the -laking is :ering and as scaling shes, and the dried :en room varnish, at 77F sually a brown, eviously ng of pign frames, ity for an trials and abrasive, taterial as has been illy, it is ver which d, can be ratio (see D 16 contrast ratio). The term covering power has no specific relationship to hiding power, and actually has no precise meaning. hue--under color of an object, see hue. hydroxy] number--the number of milligrams of potassium hydroxide (KOH) equivalent to the hydroxyl content of 1 g of sample. industrial talc--a mineral product varying in composition from that approaching the theoretical formula of talc, Mg3Si4O10 (OH)2, to mixtures of talc and other naturally associated minerals, some of which may be fibrous as defined in ASTM Definitions D 2946, Terms Relating to Asbestos. These fibrous minerals may or may not be asbestos. industrial talc, nonasbestos type--industrial talc of which less than 2 particles per 100 particles (by light microscopy) are asbestos fibers, where "asbestos fiber" is defined as being both a fiber by Definitions D 2946 and one of the asbestiform varieties of serpentine, riebeckite, cummingtonite (which are chrysotile, crocidolite and amosite, respectively), anthophyllite, tremolite, or actinolite. The nonasbestiform varieties of these same minerals are not asbestos. intumescent coating--a fire-retardant coating (which see) that when heated forms a foam produced by nonflammable gases, such as carbon dioxide and am monia. This results in a thick, highly insulating layer of carbon (about fifty times as thick as the original coating) that serves to protect the coated substrate from fire, japan--a varnish yielding a hard, glossy, dark-colored film. Japans are usually dried by baking at relatively high temperatures. japan, a vehicle for japan colors; frequently contains shellac, japan color--a paste containing pigment and a grinding japan vehicle used for lettering and decoration, japan drier--a resinate-base liquid drier, lacquer--a coating composition that is based on synthetic thermoplastic film-forming material dissolved in organic solvent that dries primarily by solvent evaporation. Typ ical lacquers include those based on nitrocellulose, other cellulose derivatives, vinyl resins, acrylic resins, etc. lake--a special type of pigment consisting essentially of an organic soluble coloring matter combined more or less definitely with an inorganic base or carrier. It is character ized generally by a bright color and a more or less pronounced translucency when made into an oil paint. Under this term are included two (and perhaps three) types of pigment: (a) the older original type composed of hydrate of alumina dyed with a solution of the natural organic color, (b) the more modem and far more exten sive type made by precipitating from solution various coal-tar colors by means ofa metallic salt, tannin, or other suitable reagent, upon a base or carrier either previously prepared or coincidently formed, and (c) a number combining both types in varying degree might be regarded as a third class. lap (coatings)--the region where one area of a coated surface merges into an adjacent freshly-coated area during appli cation of a single coat to the entire surface. cD< ( dcc< o n--The objective of the painter is to avoid showing the lap. latex paint--under paint, see latex paint, lightness--under color of an object, see lightness, maleic resin--under resin, synthetic, see maleic resin, liquid--(flammability regulations) a substance that has a definite volume but no definite form, except such given by its container. It has a viscosity of 1 X 10-3 to 1 x 103 St (l x 10~7 to 1 x 10-` m2 s~`) at KMT (40"C) or an equivalent viscosity at agreed upon temperature. (This does not include powders and granular materials.) Liquids are divided into two classes: Class A, low viscosity--a liquid having a viscosity of 1 x 10~3 to 25.00 St (1 x 10-7 to 25.00 x 10~4 m2 s~') at KMT (40C) or an equivalent viscosity at an agreed upon temperature. Class B, high viscosity--a liquid having a viscosity of 25.01 to 1 x 103 St (25.01 x 10~4 to 1 x 10~! m2 s"`) at 104F (40C) or an equivalent viscosity at an agreed upon temperature. mass color--the color, when viewed by reflected light, of a pigment-vehicle mixture of such thickness as to obscure completely the background. Sometimes called over-tone or mass-tone. mass-tone--see mass color. melamine resin--under resin, synthetic see melamine resin. metal marking resistance--the ability of a coating to with stand streaking or marking when a metal object is rubbed against or dragged across the surface of the coating, mildew (fungus) resistance (coatings)--the ability of a coating to resist fungus growth that can cause discolora tion and ultimate decomposition of a coating's binding medium. miidewstat--a chemical agent that inhibits the growth of mildew. mohair paint roller cover--a cover in which the paint applicating material is woven of short pile velour that contains wool or angora goathair. natural resin--see resin, natural. nondrying oil--an oil that does not of itself possess to a perceptible degree the power to take up oxygen from the air and lose its liquid characteristics, nonvolatile content--the portion of a coating that does not evaporate during drying or curing under specified condi tions, comprising the binder and, if present, the pigment. (The percent volatile content is obtained by subtracting the nonvolatile content from 100.) nonvolatile vehicle--the liquid portion of a paint excepting its volatile thinner and water. oil color--an oil paint containing a high concentration of colored pigment, commonly used for tinting paint. oil paint--under paint, see oil paint, oil varnish--under varnish, see oil varnish. opacity--the degree of obstruction to the transmission of visible light. In this sense "opacity" is a relative term, it being considered that given a film sufficiently thin, in paint technology at least, there is no absolutely opaque sub stance. over-tone--see mass color. 11 DUP050297194 D 16 paint vb--to apply a thin layer of a coating to a substrate by brush, spray, roller, immersion, or any other suitable means. paint n, general--a pigmented coating. See coating, paint n, specific--a classification sometimes employed to distinguish pigmented drying oil coatings ("paints") from synthetic enamels and lacquers. emulsion paint--a paint, the vehicle of which is an emulsion of binder in water. The binder may be oil, oleoresinous varnish, resin, or other emulsifiable binder. latex paint--a. paint containing a stable aqueous disper sion of synthetic resin, produced by emulsion polymeriza tion, as the principal constituent of the binder. Modifying resins may also be present. oilpaint--a paint that contains drying oil or oil varnish as the basic vehicle ingredient. paste paint--a paint in which the pigment is sufficiently concentrated to permit a substantial reduction with vehicle before use. water paint--a paint, the vehicle of which is a water emulsion, water dispersion, or ingredients that react chem ically with water. paint brush--a paint application tool consisting of a flexible brushing part composed of long filamentary material (brushing material) bound to a handle. D' e( fee< gh--Typical types include designs for varnish, enamel, sash and wall painting. They are manufactured in a range of shapes and sizes. paint brush bristle--hair ofthe swine (for example: pig, hog, boar), used in brushing material, paint brush ferrule--outer band that joins the brushing material to the handle. paint brush filament--a synthetic polymer extrusion used in brushing material. paint brush head--brush without the handle, paint brush length clear--also called "length out", the ex posed length of the brushing material from the ferrule to the tip end. paint brush thickness--measurement of the brushing mate rial across the narrow opening of the ferrule, paint pad--a paint application tool consisting of short filamentary material usually bonded to a flat, resilient backing connected to a handle designed to apply paint by a wiping action. paint roller--a complete paint application tool consisting of a roller frame and a roller cover designed to apply paint by a rolling action. paint roller core--a structural tube that forms the base ofthe roller cover to which paint applicating material is attached, paint roller cover--a tubular sleeve consisting of a paint applicating material secured to a core, paint roller cover pile height--also called "nap length"; the length of the roller cover paint applicating material from pile backing to pile face. paint roller frame--a frame and handle assembly designed to hold a roller cover. paste paint--under paint, see paste paint, penta resin--under resin, synthetic, see penta resin, phenolic resin--under resin, synthetic, see phenolic resin. picking--a rolling up in the lap (see lap) when the previously applied paint film is in a semisolid (gel-llke) state of drying causing a tacky resistance to the brush or roller and resulting in an unsightly nonuniform appearance in th* final dried film. pigment--the fine solid particles used in the preparation of paint or printing ink and substantially insoluble in the vehicle. Asphaltic materials are not pigments except when they contain substances substantially insoluble in the vehicle in which they are used. pigment volume--the percent by volume of pigment in the nonvolatile portion of a paint or printing ink, as calculated from bulking value and composition data. The letters PV are commonly used as an abbreviation. pinholes--small pore-like flaws in a coating that extend entirely through the applied film and have the general appearance of pin pricks when viewed by reflected light plasticizer--a substance added to paint, varnish, or lacquer to impart flexibility. primer--the first of two or more coats of a paint, varnish, or lacquer system. printing ink--a colored or pigmented liquid or paste compo sition that dries to a solid film after application as a thin layer by printing machinery. print resistance (coatings)--the ability of a coating to resist taking on the imprint due to the pressure of another surface placed against it. putty--a dough-like material consisting of pigment and vehicle, used for sealing glass in frames, and for filling imperfections in wood or metal surfaces. See glaring compound. resin, natural--a solid organic substance, originating in the secretion of certain plants or insects, which is thermo plastic, flammable, nonconductive of electricity; breaks with a conchoidal fracture (when hard); and dissolves in certain specific organic solvents but not water. fossil resin--a natural resin of ancient origin usually found in the earth. resin, synthetic--a synthetic substance physically similar to natural resin. acrylic resin--a synthetic resin made from derivatives of acrylic acid. alkyd resin--a synthetic resin made from polyhydric alcohols and polybasic acids; generally modified with resins, fatty oils or fatty acids. ester gum--a resin made from rosin or rosin adds and a polyhydric alcohol, such as glycerine or pentaerythritol. maleic resin--a resin made from a natural resin and maleic anhydride or maleic acid. melamine resin--a synthetic resin made from melamine and aldehyde. penta resin--ester gum made from rosin and pentaerythritol. phenolic resin--a synthetic resin made from phenols and aldehydes. styrene resin--a synthetic resin made from vinyl ben zene. urea resin--a synthetic resin made from urea and an aldehyde. vinyl resin--a synthetic resin made from vinyl com* pounds. rust (coatings)--the reddish material, primarily hydrated iron oxide, formed on iron or its alloys resulting from 12 expos white rust resi the sc saturate scaling sealer-- of fin preve semidry dryin dema shade-- surfai tially highe satun Iightr Pr desig prod> there towa by st color by e> wide adjec appa may sort, dark sheeps appl; tann size--i sorpsimi first coat indi T usag ordi appl size subs size spar v spirit r soil (c soot emb calk solid-- visci (40 tem rials sP*ead mat DUP050297195 -N rand 3 the on of a the when 1 the n the ilated rsPV xtend :neral ght. cquer sh, or >mpoi thin resist tother t and filling lazing in the ermooreaks ves in sually ilar to 'atives lydric with and a tol. 1 and from henols /I ben- md an 1 com- /drated g from # D 16 exposure to humid atmosphere or chemical attack; See white rust. rust resistance (coatings)--the ability of a coating to protect the substrate of iron or its alloys from rusting, saturation--under color of an object, see saturation. scaling resistance (coatings)--See flaking resistance, sealer--a liquid composition to prevent excessive absorption of finish coats into porous surfaces; also a composition to prevent bleeding (see size). semidrying oil--an oil that possesses the characteristics of a drying oil but to a lesser degree. There is no definite line of demarcation between drying and semidrying oils, shade--a term descriptive of a lightness difference between surface colors, the other attributes of color being essen tially constant. A lighter shade of a color is one that has higher lightness but approximately the same hue and saturation; and a darker shade is one that has a lower lightness. Primarily, the term "shade" is derived from shadow and designates a change in appearance analogous to that produced by a local reduction in illumination. It should, therefore, when strictly used, express only the change toward a darker color. Shade of a color has been defined by several authorities as the mixture of black with that color, thus establishing its opposite character to "tint," but by extension of its relative sense it has been frequently and widely used to include lighter shades by use of the adjective "lighter" or "paler." Although such expressions apparently involve a contradiction, it is clear that while we may have a shade of a color or darker color of the same sort, it is easy to conceive of another shade not quite so dark and therefore lighter. sheepskin paint roller cover--a cover in which the paint applicating material is wool fleece still attached to its tanned natural skin. size--usually a liquid composition to prevent excessive ab sorption of all paints into plaster, old wall paint, and similar porous surfaces; also a liquid composition used as a first coat on metal to improve adhesion of succeeding coats (latter usage is limited to the metal decorating industry). The terms sealer and size are almost synonomous, but usage has established certain differences. A sealer is ordinarily a thin varnish or clear lacquer and is usually applied on wood and metal surfaces. Ordinary painter's size is a thin solution of glue, starch or other water-soluble substance and is usually applied on piaster surfaces, but size used in metal decorating is a thin varnish. spar varnish--under varnish, see spar varnish, spirit varnish--under varnish, see spirit varnish. soil (coatings)--disfiguring foreign materials such as dirt, soot, or stain, other than microorganisms, deposited on or embedded in a dried film of applied coating material; also called dirt. solid--(flammability regulations) a substance that has a viscosity greater than 1 x tO3 St (1 x 10-1 m2 s_1) at 104F (40C) or an equivalent viscosity at an agreed upon temperature. (This includes powders and granular mate rials.) spreading rate--the area covered by a unit volume of coating material frequently expressed as square feet per gallon. stain--a discoloration, arising from foreign materials, that penetrates into the coating. stain--a penetrating composition that changes the color of a surface, usually transparent and leaving practically no surface film. styrene resin--under resin, synthetic, see styrene resin. surfacer--a pigmented composition for filling minor irregu larities to obtain a smooth uniform surface preparatory to applying finish coats; usually applied over a primer and sandpapered for smoothness. synthetic paint roller cover--a cover in which the paint ap plicating material is man-made material. synthetic resin--see resin, synthetic. talc--see industrial talc and industrial talc, nonasbestos type, temporary coating--a coating designed to protect or decorate a substrate for a limited time that can be readily removed either by mechanical or chemical means, thinner--the portion of a paint, varnish, lacquer, or printing ink, or related product that volatilizes during the drying process. tint--a color produced by the mixture of white pigment or paint in predominating amount with a colored pigment or paint, not white. The tint of a color is, therefore, much lighter and much less saturated than the color itself, tinting strength--the power of coloring a standard paint or pigment. toner--an organic pigment that does not contain inorganic pigment or inorganic carrying base, undertone--the colouxtf a thin layer of pigment-vehicle mixture applied on a white background. urea resin--under resin, synthetic, see urea resin. urethane coatings--coatings based upon vehicles containing a minimum of 10 percent by weight (nonvolatile vehicle basis) of a polyisocyanate monomer reacted in such a manner as to yield polymers containing any ratio, propor tion or combination of urethane linkages, active isocyanate groups, or polyisocyanate monomer. The reac tion products may contain excess isocyanate groups avail able for further reaction at time of application or may contain essentially no free isocyanate as supplied. Type I, one-package prereacted--urethane coatings characterized by the absence of any significant quantity of free isocyanate groups. They are usually the reaction product of a polyisocyanatc and a polyhydric alcohol ester of vegetable oil acids and are hardened with the aid of metallic soap driers. Type II, one-package moisture cured--urethane coat ings characterized by the presence of free isocyanate groups and capable of conversion to useful films by the reaction ofthese isocyanate groups with ambient moisture. Type III, one-package heat cured--urethane coatings that dry on cure by thermal release of blocking agents and regeneration of active isocyanate groups that subsequently react with substances containing active hydrogen groups. Type IV, two-package catalyst--urethane coatings that comprise systems wherein one package contains a prepoly mer or adduct having free isocyanate groups capable of forming useful films by combining with a relatively small quantity of catalyst, accelerator, or crosslinking agent such as a monomeric polyol or polyamine contained in a 13 DUP050297196 D 16 second package. This type has limited pot-life after the two vernonia ofl--a low-viscosity epoxidized drying oil from the components are mixed. Type V, two-package polyol--urethane coatings that comprise systems wherein one package contains a prepol ymer or adduct or other polyisocyanate capable of forming useful films by combining with a substantial quantity of a second package containing a resin having active hydrogen groups with or without the benefit of catalyst. This type has limited pot-life after the two components are mixed. Type VI, one-package nonreactive lacquer--urethane solution coatings characterized by the absence of any significant quantity of free isocyanate or other functional seed of an African plant, Vernonia galamensis, containing three reactive epoxy groups and three carbon--carbon double bonds per triglyceride molecule and is character ized by its very low viscosity and melting point. DISCUSSION--It flows easily even at temperatures below 0C and thus needs only a fraction of the volatile solvents usually used for other drying oils. Thus, it can be used as a reactive diluent for high solids alkyds and epoxy coating formulations. vinyl resin--under resin, synthetic, see vinyl resin, volatile thinner--see thinner. volume percent solids--the portion of a coating that remains as part of the dry film expressed as percent by volume. 4> groups. Such coatings convert to solid films primarily by solvent evaporation. iD< ( jii< kl--This contrasts to another convention of expressing solids content by weight percent. Often a percent is given without varnish--a liquid composition that is converted to a trans parent or translucent solid film after application as a thin specifying whether it is volume or weight. This is confusing and leads to errors in coating calculations. layer. water paint--under paint, see water paint. bituminous varnish--a dark-colored varnish containing wet adhesion--the ability of a coating film to adhere tightly bituminous ingredients. The varnish may be either of the to the substrate directly beneath it under wet conditions oil or spirit type. oil varnish--a varnish that contains resin and drying oil such as rain, dew, washing, etc. wet storage stain (coatings)--See white rust, white rust--white corrosion products (zinc hydroxide and as the basic film-forming ingredients and is converted to a zinc oxide) on zinc-coated articles. They form when the t solid film primarily by chemical reaction. spar varnish--a varnish for exterior surfaces. The name originated from its use on spars of ships. parts are stored so close together that condensed moisture is entrapped between them and the air circulation is inadequate to assist drying. Also called wet storage stain. 1. Scot spirit varnish--a varnish that is converted to a solid film See rust. 1.1 " primarily by solvent evaporation, zinc-rich primer--a primer for ferrous metals, incorporating petrolei vehicle--the liquid portion of a paint or printing ink. zinc dust at a concentration sufficient to make the dried the dis Anything that is dissolved in the liquid portion of a paint film electrically conductive thus providing cathodic pro during or printing ink is a part of the vehicle. tection to the ferrous substrate. Table D 244. D 400( This standard Is subject to revision at any lime by the responsible technicalcommittee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments are Invited either for revision of this standard or toradditional standards previoi 2560,1 and should be addressed to ASTM Headquarters. Your comments will receive careiul consideration at a meeting ot the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. Nmn' from A ASTM 1.2 ations addre. the re approi applic specif; 1.3 stands 2. Re: 2.1 D8D2 14 DUP050297197 from the attaining --carbon haracter- v 0C and y used for it for high remains tame. expressing :n without ; and leads re tightly editions xide and vhen the moisture lation is ige stain. rporating the dried " die pro- Designation: D 95 - 83 (Reapproved 1990)e1 Designation MPMS Chapter 10.5 Designation 74/82 An American National Standard British Standard 4385 American Association State Highway Transportation Standard AASHTO No. T55 Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation1 This standard is issued under the fixed designation D 95; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This lest method has been approved by the sponsoring committees and accepted by the cooperating organizations in accordance with established procedures. This test method has been approvedfor use by agencies ofthe Department ofDefense andfor listing in the DoD Index ofSpecifications and Standards. 41 Nop' --Paragraphs 1.3 and 11.2 were added editorially in May 1990. 1. Scope 1.1 This test method covers the determination of water in petroleum products, tars, and other bituminous materials by the distillation method. The specific products considered during the development of this test method are listed in Table 1. For bituminous emulsions refer to Test Method D 244. This test method, along with ASTM Test Method D 4006 (API Chapter 10.2 and IP 358), supersedes the previous edition of ASTM Test Method D 95 (API Standard 2560, IP 74). NOTE i--With some types ofoil, satisfactory results may be obtained from ASTM Test Method D4007 (API Chapter 10.3, IP 358, and ASTM Method D 1796 API Chapter 10.6). 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see 5.1.1.2 and 5.1.1.3. 1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only. 2. Referenced Documents 2.1 ASTM Standards: D86 Method for Distillation of Petroleum Products2 D 244 Test Methods for Emulsified Asphalts3 1 This test method is under the jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and API Committee on Petroleum Measure ment and is the direct responsibility of Subcommittee D02.02 on Joint ASTM-API Committee on Static Petroleum Measurement. Current edition approved March 25, 1983. Published January 1984. Originally Published as D 95.21. Last previous edition D 95 - 70 (1980). 2 Annual Book ofASTM Standards. Vols 05.01 and 06.03. 3 Annual Book ofASTM Standards. Vol 04.03. D1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)4 D4006 Test Method for Water in Crude Oil by Distillation5 D4007 Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)5 D4057 Practice for Manual Sampling of Petroleum and Petroleum Products5 D4177 Method for Automatic Sampling of Petroleum and Petroleum Products5 E 123 Specification for Apparatus for Determination of Water by Distillation5 2.2 API Manual ofPetroleum Measurements Standards:6 Chapter 8.1 Manual Sampling of Petroleum and Petro leum Products (ASTM Practice D 4057) Chapter 8.2 Automatic Sampling of Petroleum and Petro leum Products (ASTM Test Method D 4177) Chapter 10.2 Determination of Water in Crude Oil by the Distillation Method (ASTM Test Method D 4006) Chapter 10.3 Determination of Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Proce dure) (ASTM Test Method D 4007) Chapter 10.6 Determination of Water and Sediment in Fuel Oil by the Centrifuge Method (ASTM Test Method D 1796) 2.3 British Standard:1 756 Dean and Stark Apparatus 3. Summary of Test Method 3.1 The material to be tested is heated under reflux with a * Annual Book ofASTM Standards, Vol 05.01. 5 Annual Book ofASTM Standards, Vol 05.03. 6 Available from American Petroleum Institute, 1220 L St, N.W., Washington, DC 20005. 7 Available from American National Standards Institute, 13th Floor, 11 W. 42nd Street, New York, NY 10036. 15 DUP050297198 D 95 TABLE 1 Type of Solvent-Carrier Liquid Versus Material to be Tested Type of Solvent-Carrier Liquid Material to be Tested Aromatic Petroleum distillate Volatile spirits asphalt, tar, coal tar, water gas tar, road tar, cutback bitumln, liquid asphalt tar acid road oil. fuel oil, lubricating oil, petroleum sulfonates lubricating grease water-immiscible solvent, which co-distills with the water in the sample. Condensed solvent and water are continuously separated in a trap, the water settling in the graduated section of the trap and the solvent returning to the still. 4. Significance and Use 4.1 A knowledge of the water content of petroleum products is important in the refining, purchase, sale, and transfer of products. 4.2 The amount of water as determined by this method (to the nearest 0.05 volume %) shall be used to correct the volume involved in the custody transfer of oil. FIG. 2 Two-millilitre Receiver Showing Alternative Connections to Glass Still 5. Solvent-Carrier Liquid 5.1 A solvent-carrier liquid appropriate to the material being tested (see Table 1) shall be used. 5.1.1 Aromatic Solvent--The following aromatic solvents are acceptable: 5.1.1.1 Industrial Grade Xylene. 5.1.1.2 A blend of 20 volume % industrial grade toluene and 80 volume % industrial grade xylene (Warning--Flam mable. Vapor harmful. See Annex AI.l.) 5.1.1.3 Petroleum or Coal Tar Naphtha (Warning--Ex tremely flammable. Harmful if inhaled. Vapors may cause fire. See Annex), free of water, yielding not more than 5% distillates at 125C (257F) and not less than 20% at 160C (320F) when tested by Method D 86 and with a relative density (specific gravity) not lower than 0.8545 at 15.56/ 15.56'C (60/60'F). 5.1.2 Petroleum Distillate Solvent--A petroleum distillate FIG. 1 Typical Assembly with Glass Still (Dean and Stark) solvent, 5% boiling between 90' and 100'C (194' and 212'F) and 90% distilling below 210'C (410F), shall be used. 5.1.3 Volatile Spirits Solvent--The following volatile spirits solvents are acceptable: 5.1.3.1 Petroleum Spirit, with a boiling range of 100' to 120C (212' to 248'F). 5.1.3.2 Isooctane, of 95% purity or better. 6. Apparatus 6.1 General--The apparatus comprises a glass or metal still, a heater, a reflux condenser, and a graduated glass trap. The still, trap, and condenser may be connected by any suitable method that produces a leakproof joint Preferred connections are ground joints for glass and O-rings for metal to glass. Typical assemblies are illustrated in Figs. 1,2, and 3. The stills and traps should be chosen to cover the range of materials and water contents expected. 6.2 Still--A glass or metal vessel with a short neck and suitable joint for accommodating the reflux tube of the trap shall be used. Vessels of 500, 1000, and 2000-mL nominal' capacity have proved satisfactory. 6.3 Heater--A suitable gas burner or electric heater may be used with the glass still. A gas ring burner with ports on the inside circumference shall be used with the metal stilL The gas ring burner shall be of such dimensions that it may be moved up and down the vessel when testing materials that are likely to form or solidify in the still. 6.4 Glassware--Dimensions and descriptions of typical glassware for use in this method are provided in Specification E 123 and British Standard 756. A straight water-cooled condenser with a length of 400 mL is recommended in place of the length of 300 mL specified in British Standard 756. qrN ' 2--Instead of standardizing on a particular apparatus specifi cation with respect to dimensions and style, a riven apparatus will be deemed satisfactory when accurate results are obtained by the standard- addition technique described in Section 7. 7. Standardization 7.1 A given assembly of apparatus will be considered 1 16 DUP050297199 D 95 sns 2"F) atile i0 to letal rap. any rred letal id 3. ,e of and rap nal nay on still. may that pical ition oled )lace 56. lecifiill be idard lered FIQ. 3 Typical Assemblies with Metal Still satisfactory when accurate readings are obtained from the addition of known amounts of water from a calibrated buret or pipet to a clear hydrocarbon oil and tested in accordance with Section 9. 7.2 The readings shall be judged accurate if the permis- TABLE 2 Permissible Limits in Millilitres Capacity of Receiver at 20C Volume of Water Added to Flask at 20'C Permissible Limits for Recovered Water at 20C 21 10 1 10 5 25 12 1 0.05 1 0.1 5 0.2 12 0.2 sible limits given in Table 2 for the various sized graduated traps are not exceeded. 7.3 A reading outside the permissible limits suggests a malfunction resulting from vapor leaks, too rapid boiling, inaccuracies in calibration of the trap, or ingress of extra neous moisture. Eliminate these factors before repeating the standardization. 8. Sampling 8.1 Sampling is defined as all steps required to obtain an aliquot ofthe contents of any pipe, tank, or other system and to place the sample into the laboratory test container. Only representative samples obtained as specified in Practice D 4057 (API Chapter 8.1) and Method D 4177 (API Chapter 17 DUP050297200 8.2) shall be used for this test method. 8.2 The size of the test portion should be based on the expected water content of the sample, such that the water yield does not exceed the capacity of the trap (unless a trap with a stopcock is used since excess water can be withdrawn into a graduated cylinder). 9. Procedure 9.1 Measure a suitable amount of sample to an accuracy of 1 % and transfer it to the still. 9.2 Measure ordinary liquid samples in a graduated cyl inder of an appropriate size. Rinse the material adhering to the cylinder with one 50-mL and two 25-mL portions of the solvent-carrier liquid (see Section 5 and Table 1). Drain the cylinder thoroughly after the sample transfer and each rinsing. 9.3 Weigh solid or viscous materials directly into the still and add 100 mL of the selected solvent-carrier liquid. In cases of material with a low-water content when large samples must be used, a solvent-carrier liquid volume in excess of 100 mL may be necessary. 9.4 Glass beads or other boiling aids may be added, if necessary, to reduce bumping. 9.5 Assemble the components of the apparatus as illus trated in Figs. 1, 2, and 3 choosing the trap in accordance with the expected water content of the sample and making all connections vapor and liquid tight. If a metal still with a removable cover is used, insert a gasket of heavy paper, moistened with solvent, between the still body and the cover. The condenser tube and trap must be chemically dean to assure free drainage of water into the bottom of the trap. Insert a loose cotton plug in the top of the condenser to prevent condensation of atmospheric moisture inside it. Circulate cold water through the jacket of the condenser. 9.6 Apply heat to the still, adjusting the rate of boiling so that condensed distillate discharges from the condenser at the rate of 2 to 5 drops per second. If the metal still is used, start heating with the ring burner about 76 mL (3 in.) above Type Repeatability Reproducibility TABLE 3 Water Col lected, mL 0.0-1.0 1.1-25 0.0-1.0 1.1-25 Precision Difference, mL 0.1 0.1 or 2 % of the mean, whichever Is greater 0.2 0.2 or 10 % of the mean, whichever is greater the bottom of the still and gradually lower the burner as the distillation proceeds. Continue distillation until no water is visible in any part ofthe apparatus except in the trap, and the volume of water in the trap remains constant for 5 min. if there is a persistent ring of water in the condenser tube carefully increase the rate of distillation or cut off the condenser water for a few minutes. 9.7 When the evolution of water is complete, allow the trap and contents to cool to room temperature. Dislodge any drops of water adhering to the sides of the trap with a glass rod or other suitable means and transfer them to the water layer. Read the volume of the water in the trap to the nearest scale division. 10. Calculation 10.1 Calculate the water in the sample, as weight or volume percent, in accordance with the basis on which the sample was taken, as follows: Water, % = V/W x 100 where: V = volume of water in trap and W = weight (or volume of sample). Volatile water-soluble material, if present, may be measured as water. 10.2 Report the results as the water content to the nearest 0.05% if the 2-mL receiver has been used and to the nearest 0.1% if the 10-mL or 25-mL receiver has been used with a 100-mL or 100-g sample. 11. Precision and Bias 11.1 Precision--The criteria described in Section 11.1.1 and 11.1.2 should be used to judge the acceptability of results (95% probability) when using the 10-mL or 25-mL traps. The precision when using the 2-mL trap has not been established. 11.1.1 Repeatability--The difference between successive test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material, would, in the long run, in the normal and correct operation of the test method, exceed the values in Table 3 in only one case in twenty. 11.1.2 Reproducibility--The difference between two single and independent test results obtained by different operators working in different laboratories on identical test material, would, in the long run, in the normal and correct operation of the test method, exceed the values in Table 3 in only one case in twenty. 11.2 Bias--A bias statement is under development. ; i \ ! I Al.l X Warn Keep Keep Use v Avoir Avoie Al.2 N Warn Harm ; 18 DUP050297201 as the /ater is indthe min. If r tube, iff the ow the Ige any a glass : water nearest ght or ich the :asured nearest nearest with a 11.1.1 results . traps, t been cessive t same lentical al and 'ues in two Terent al test orrect le 3 in t. D9S ANNEX (Mandatory Information) Al. PRECAUTIONARY STATEMENTS Al.l Xylene/Toluene Warning--Flammable. Vapor harmful. Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid breathing of vapor or spray mist. Avoid prolonged or repeated contact with skin. AI.2 Naphtha Warning--Extremely flammable. Harmful if inhaled. Vapors may cause flash fire. Keep away from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid a build-up of vapors and eliminate all sources of ignition, especially nonexplosion proof electrical apparatus and heaters. Avoid prolonged breathing of vapors or spray mist. Avoid prolonged or repeated skin contact. The American Society for Testing and Materials takes no position respecting the validity of any patent rights assorted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either tor revision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 19 DUP0502 97202 <1 Designation: D 154 ~ 85 (Reapproved 1989)e1 Standard Guide for Testing Varnishes1 This standard is issued under the iixed designation D 154; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. " Nst' --Editorial changes made throughout in October 1989. 1. Scope 1.1 This guide covers the selection and use of procedures for testing varnishes. Some test methods are included but most sections refer to specific ASTM test methods. 1.2 Varnishes may be applied under such diverse condi tions to so many different surfaces, and their dried films may be subjected to so many kinds of wear and exposure, that it is not possible to assure desired performance from a single selection oftest methods and numerical results. Those skilled in varnish technology may find partial assurance of ob taining desired qualities in various types of varnishes through careful selection of the methods covered and intelligent interpretation of results. 1.3 This standard may involve hazardous materials, oper ations and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 56 Test Method for Flash Point by Tag Closed Tester2 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester2 D445 Test Method for Kinematic Viscosity of Trans parent and Opaque Liquids (and the Calculation of Dynamic Viscosity)3 D479 Test Method for Reactivity of Paint Liquids4 D 523 Test Method for Specular Gloss5 D658 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive5 D968 Test Method for Abrasion Resistance of Organic Coatings by Falling Abrasive5 D1200 Test Method for Viscosity by Ford Viscosity Cup5 D1209 Test Method for Color of Clear Liquids (PlatinumCobalt Scale)6 1 This guide is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.33 on Polymers and Resins. Current edition approved May 31, 1985. Published July 1985. Originally published as D 154 - 23. Last previous edition D 154 - 76. 2 Annual Book of ASTM Standards, Vols 05.01 and 06.03. 3 Annual Book ofASTM Standards, Vols 05.01 and 10.03. 4 Discontinued; see 1983 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vol 06.01. 6 Annual Book ofASTM Standards, Vols 05.01 and 06.03. D1310 Test Method for Flash Point and Fire Point of Liquids by Tag Open-Cup Apparatus6 D1469 Test Method for Total Rosin Acids Content of Coating Vehicles7 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products5 D 1542 Test Method for Qualitative Detection of Rosin in Varnishes8 D 1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)9 D 1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method9 D 1546 Test Method for Performance Tests of Clear Floor Sealers5 D1639 Test Method for Acid Value of Organic Coating Materials5 D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature5 D1641 Test Method for Exterior Durability of Varnishes5 D1644 Test Methods for Nonvolatile Content of Var nishes5 D1647 Test Method for Resistance of Dried Films of Varnishes to Water and Alkali5 D1729 Practice for Visual Evaluation of Color Difference of Opaque Materials10 } D2090 Test Method for Clarity and Cleanness of Paint ` Liquids11 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates5 D 2369 Test Method for Volatile Content of Coatings5 D2805 Test Method for Hiding Power of Paints by Reflectometry5 1 ; j D3278 Test Methods for Flash Point of Liquids by | Setaflash Closed-Cup Apparatus12 j D 3964 Practice for Selection of Coating Specimens for | Appearance Measurement5 D 4039 Test Method for Reflection Haze of High Gloss | Surfaces5 j D4060 Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser5 E 308 Method for Computing the Colors of Objects by Using the CIE System10 ; ; | ! 7 Annual Book ofASTM Standards, Vol 06.02. 8 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 9 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 10 Annual Book ofASTM Standards, Vol 14.02. 11 Annual Book ofASTM Standards, Vols 06.02 and 06.03. 12 Annual Book ofASTM Standards, Vol 06.03. 3. aes filn liqi acc 4. < 4 coI< the blei exp colt isor Tes 4 usir in a 4 trist lO-i E3< 5. ' 5. imp tion as h coat Vise 5. cosh Test inC ofT 5 cosi effli 5. vise 6. S 6. of a the \ temp (25< Met! weig; 7. V 7.1 amoi atmo pend to va surro 20 DUP050297203 >int of tent of 1, Lac- osin in liquids liquids r Floor boating Formanishes5 )f Varilms of Terence f Paint irences s5 igs5 its by ids by tens for h Gloss Organic jects by D 154 LIQUID VARNISH PROPERTIES TABLE 1 List of Test Methods 3. Appearance Test Method Section ASTM Designation 3.1 Appearance ofthe liquid varnish is important both for aesthetic reasons and because it indicates whether the dried film is likely to have a satisfactory appearance. Examine the liquid varnish for foreign matter, sediment or skins in accordance with Test Method D 2090. 4. Color 4.1 Most varnishes are predominantly yellow but the color ofthe liquid varnish is only a preliminary indication of the color of the dried varnish film. The initial color may bleach or may darken depending upon the conditions of exposure. Determine approximately and quickly the liquid color of small specimens in Gardner-Holdt tubes by compar ison with the Gardner Color Standards in accordance with Test Method D 1544. 4.2 Measure the color of extremely pale varnishes by using larger specimens in 100-mL cylinders, 300 mm deep, in accordance with Test Method D 1209. Liquid Varnish Properties: Appearance Color (Gardner) Color, Platinum-Cobalt Scale Color, tristimulus Viscosity: Bubble time (Gaidner-Holdt) Ford cup efflux Kinematic, high precision Specific gravity Volatile content Nonvolatile matter Flash point: Tag closed-cup PensKy Martens Tag open-cup Setaflash closed tester Skinning Add value Reactivity of paint liquids Rosin content, quantitative Rosin content qualitative (Ueberman-Storch and Halphert-Hlcks) 3 4.1 4.2 4.3 5 5.2 5.3 5.4 6.7 7 8 9 10 11 12 13 13 D 2090 D 1544 D 1209 E308 01545 D 1200 D 445 D 1475 0 2369 D1644 D 56 D 93 D 1310 D 3278 D1639 D479 D1469 D1542 4.3 A more precise measure of color, in terms of tristimulus values, may be made on small specimens in 10-mm cells with parallel walls in accordance with Method Drying and Curing Properties: Drying time Print free time 14 D 1640 15 D1640 E 308. 5. Viscosity 5.1 The viscosity of a varnish or clear vehicle is a property important in ease of application; varnishes for brush applica tion are typically 1 to 2 St whereas varnishes with viscosities as high as 100 St may sometimes be added to lithography coatings or used as mixing vehicles for producing enamels. Viscosity is commonly measured at 77F (25C). 5.2 For the rapid, approximate measurement of the vis cosity of transparent varnishes, determine the bubble time by Dry Vernlsh Properties: Gloss: Specular gloss Reflective haze Resistance of dried films to water and alkali Abrasion resistance: Carborundum air blast Falling abrasive Taber abraser Exterior durability Color of dried film 16 17 13 19 20.1 20.2 D523 04039 D 1647 D658 D968 D 4060 D1641 D 2244 D1729 Test Method D 1545. Report the viscosity either in stokes or in Gardner-Holdt letter designations as described in Table 1 Clear floor sealers 21 D1546 of Test Method D 1545. 5.3 For a rapid, approximate measurement of the vis Method D 2369 be used to determine the volatile content of cosity of translucent varnishes, determine the Ford cup a varnish. efflux time in accordance with Test Method D 1200. 5.4 For the precise measurement of viscosity, use capillary 8. Nonvolatile Matter viscometers as described in Test Method D 445. 8.1 Nonvolatile content is an indication of the amount of 6. Specific Gravity ! 6.1 Specific gravity of a varnish is the ratio of the weight permanent film-forming material contained in a varpish. The normal drying of a varnish film may involve varying amounts ofabsorption of oxygen from the air, loss ofvolatile ; of a given volume of the varnish at a given temperature to solvents, and continuing decomposition of the dried film. ' the weight of an equal volume of distilled water at the same The net result of this process may differ somewhat from a temperature. Determine specific gravity or density at 77'F nonvolatile determination at a temperature higher than the (25C) or other agreed temperature in accordance with Test normal drying conditions. Method D 1475 which allows use ofeither a pycnometer or a 8.2 With due regard to the composition of the varnish, 1 weight per gallon cup. determine the nonvolatile matter in accordance with either Method A (3 h at 220F (lC^C)) or Method B (10 min at 1 7. Volatile Content ; 7.1 Volatile matter determination is an indication of the | amount of material in the coating that will be given offto the J atmosphere in the area where the coating is applied. De- 300F (149C)) of Test Methods D 1644. 8.3 As noted in Test Method D 2369, nonvolatile matter can also be calculated by subtracting the volatile content from 100. ! pending upon the method of application, the time required to vaporize the volatile and the conditions ofthe atmosphere 2 surrounding the application, it is recommended that Test 9. Flash Point 9.1 Determine the flash point of varnishes having a DUP050297204 viscosity ofless than 9.5 cSt at 77T (25C) (45 SUS at 100'F) by Test Method D 56, and of varnishes having a viscosity of more than 9.5 cSt at 77F by Test Methods D 93. Alterna tively, use Test Methods D 3278, which gives comparable results to Test Methods D 56 and D 93, and Test Method D 1310. Nuv' --Due to various U.S. Government and State regulations, it is now necessary to check with appropriate departments to determine which ASTM Test Method is applicable. 10. Skinning 10.1 Varnishes, which dry by oxidation, may form a skin in a partially filled can or in a filled can that is stored for a long time. Since skins are insoluble in the varnish, they must be removed before use ifa satisfactory film is to be obtained. Use the following test to determine if a varnish has an objectionable tendency to early skin formation: 10.1.1 Container--A wide-mouth jar with a capacity of 8-fluid oz (235 mL) and dimensions of 4l/i in. (115 mm) in height and 2 in. (50 mm) in diameter. 10.1.2 Procedure--Measure a 6-fluid oz (180-mL) spec imen of the varnish into the glass container. Screw the cover on tightly, invert the jar, and leave in an inverted position, at rest, and in the dark (placing under a box or in a drawer is satisfactory). Examine the varnish for skinning at specified time intervals. 11. Acid Value 11.1 The acid value of a varnish is an indication of reactivity with basic pigments and, within any one type of composition, may indicate conformity to a standard method of preparation. It is not a general criterion of excellence in a protective coating. 11.2 Determine the acid value in accordance with Test Method D 1639. 12. Reactivity of Paint Liquids 12.1 Reactivity of a varnish with zinc oxide is a partial indication ofthe stability of the consistency ofenamels made from it and various basic pigments. 12.2 Determine the reactivity in accordance with Test Method D 479. 13. Rosin Content 13.1 Improper use of rosin and its derivatives is some times associated with inferior performance of varnishes containing them. Qualitative tests for rosin may be employed to detect the use of a significant amount in varnishes. Quantitative determination of rosin may be used to control rosin content within limits agreeable to the purchaser and the seller. 13.2 Determine the rosin content quantitatively in ac cordance with Test Method D 1469 and qualitatively with Test Method D 1542. DRYING AND CURING PROPERTIES 14. Drying Time 14.1 Small variations in film thickness, air temperature and humidity, and exposure to light and other radiation may affect drying times by 5 %. 14.2 Determine the drying stages appropriate to the var nish under test in accordance with the applicable sections of Test Methods D 1640. IS. Print-Free Time 15.1 Varnishes intended for floors, furniture, etc., are expected to bear heavy objects for long periods without marring of the surface or adhering to the object. 15.2 Determine the print-free time in accordance with that section of Test Methods D 1640. DRY VARNISH PROPERTIES 16. Gloss 16.1 Because varnishes are transparent or translucent, gloss must be measured on films applied to a nonreflecting substrate. The usual material is plane, black glass as de scribed in Test Method D2805 and similar to the gloss standards used in Test Method D 523. Gloss measurements of varnishes on wood substrates are generally not valid because the reflectance of the substrate can affect the result, but comparative tests in one laboratory of different varnishes on the same substrate may be helpful. 16.2 Gloss is usually measured in accordance with Test Method D 523 using 60" geometry. For greater sensitivity in evaluating high gloss varnishes, the 20 geometry may be used or Test Method D 4039 which uses both 20 and 60` geometries. 16.3 Prepare specimens in accordance with Practice D 3964, applying the varnish to black glass panels with a film applicator that has a clearance of 3 mils (75 pm) for varnishes with a nonvolatile content of 35 % or more and 6 mils (150 pm) for those with a nonvolatile content less than 35%. 16.4 Allow the films to dry under the conditions specified in Test Methods D 1640 for at least 24 h. For a rapid control test the films may be force dried at 120F (50C) for 1 h, providing it has been established that heat acceleration does not affect the gloss of the varnish. 16.5 Measure the gloss in accordance with Test Methods D 523 or D 4039 and report. 17. Resistance of Dried Films to Water and Alkali 17.1 Performance of varnish films is indicated in part by measurement of resistances of their dried films to water, alkali, and other reagents. 17.2 Determine the resistance to water and alkali in accordance with Test Method D 1647. 18. Abrasion Resistance 18.1 The durability and general performance of varnish films on floors' is influenced by many factors such as mechanical properties, film thickness, and exposure to light cleaning materials, various types of soil, and foot or vehicular traffic, so that no one set of tests are adequate to ensure universally satisfactory service. 18.2 An indication of the resistance to abrasion in sendee may be determined by Test Methods D 658, D 968, D 4060. All these test methods are suitable for interlabora? tory use only when results are compared by of numerical values. 22 19. I 19. expos other prelir 19. Test 20. ( 20. than color evalu D 22and a 20. is avi visua DUP050297205 the vartions of Sc., are without ice with lslucent, effecting s as dehe gloss trements ot valid te result, 'amishes nth Test itivity in may be and 60 Practice ith a film pm) for >re and 6 less than specified d control for 1 h, tion does Methods D 154 19. Exterior Durability 19.1 Durability of varnish films varies so widely with exposure to varying conditions of atmosphere and light or other radiation, that any one set of conditions is only a preliminary indication of general durability. 19.2 Determine the exterior durability in accordance with Test Method D 1641. 20. Color of Dried Film 20.1 The color of the dry film is usually more significant than that of the liquid varnish in establishing whether the color of a varnished object will be acceptable, This can be evaluated by determining, in accordance with Test Method D 2244, the color difference of white structural glass before and after application and drying of a varnish film. 20.2 If a varnish with a dry color known to be satisfactory is available, a standard panel can be prepared and used for visual color comparison in accordance with Practice D 1729. 21. Clear Floor Sealers 21.1 Clear floor sealers are varnishes of relatively low viscosity for application to wooden or other porous surfaces and are variously used as either the sole coating or for making the substrate more uniform for application of wax, varnish, or other coatings. 21.2 Evaluate clear floor sealers in accordance with Test Method D 1546. 22. Precision 22.1 No specific precision statement is made for this guide since this information is included in the referenced methods, if available. 23. Keywords 23.1 drying and curing properties; varnish acid value; varnish flash point; varnish nonvolatile contents; varnish physical properties; varnish specific gravity; varnish volatile contents; varnish viscosity The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard era expressly advised that determination of the validity of any such patent rights, and the risk ot infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every tlve years and if not revised, either reapproved or withdrawn. Your comments are invitedeither for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 RaceSt., Philadelphia, PA 19103. part by o water, alkali in >f varnish such as e to light, or vehicto ensure in service D 968, or iterlaborang instead DUP050297206 I Designation: D 185 - 84 (Reapproved 1989)e1 Standard Test Methods for Coarse Particles in Pigments, Pastes, and Paints*1 This standard is issued under the fixed designation D 185; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies ofthe Department of Defense to replace Methods 4091. 4101 ofFederal Test MethodStandard No. 141. Consult the DoD Index ofSpecifications and Standardsforthespecific year ofissuetvhich has been adopted by the Department ofDefense. I Nwx' --Editorial changes were made throughout in March 1989. 1. Scope U These test methods cover the determination of the amount of coarse particles in dry pigments and of coarse particles and skins in mixtures of pigments and vehicles. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this' standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: Ell Specification for Wire-Cloth Sieves for Testing Purposes2 3. Significance and Use 3.1 In production of paints, smoothness of the paint film is of paramount importance. Agglomerates or coarse parti cles larger than 45 pm are difficult to disperse and may prevent obtaining a smooth film. These test methods are a valuable quality control test for grading raw materials. 4. Apparatus 4.1 The apparatus shall consist of a 3-in. (75-tnm) 45-pm (No. 325) sieve conforming to Specification E It. A 3-in. 45-pm sieve for comparison purposes should be retained in the laboratory as a reference standard. Whenever a new sieve is secured, a practical test of its accuracy should be made by running on it and on the reference standard sieve a compar ison test, using a pigment that has a considerable amount of coarse particles. A reserve stock of such a pigment should be kept for this purpose. 5. Procedure for Insoluble Dry Pigments, Except Metallic Aluminum and Bronze Powders 5.1 Dry the sieve in an oven at 1.05 2'C, cool, and then 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.31 on Pigment Specifications. Current edition approved Oct. 26, 1984. Published December 1984. Originally published as D 185 - 37. Last previous edition D 185 - 78. 1 Annual Book ofASTM Standards, Vol 14.02. weigh on an analytical balance, recording the weight to 1 mg. 5.2 Weigh a specimen (25 g for basitj carbonate and basic sulfate white leads, 25 g for red lead and mercuric oxide, 2 g for black pigments of low specific gravity, 3 g for Prussian blues and graphite, and 10 g for all other pigments) of the pigment to be tested on an analytical balance to 1 mg. Wet the sieve on both sides with alcohol and transfer the specimen of pigment to the sieve and wet with alcohol. 5.3 Hold the sieve under a tap delivering about 300 to 500 mL ofthe wash liquid (water) per minute. By slightly shaking the sieve, the pigment will be rapidly carried through. A soft cameTs-hair brush may be used in aiding the operation. If the sieve is held at a slight angle so that the pigment gradually collects at one edge during the washing process, and then rotated, the pigment may be brushed out rapidly, with no risk of clogging the sieve. 5.4 After most ofthe finely divided portion of the pigment has passed through the sieve (from 2 min to 1 h, according to the kind of pigment), place the sieve in an 8-in. (200-mm) porcelain dish containing 250 mL of the wash liquid so that the sieve is covered to a depth of about 'A in. Brush the pigment remaining on the sieve with a soft 1-in. (25-mm) camel's-hair brush at the rate of two strokes per second during two periods of 10 s each. Raise the sieve from the dish after each 10-s period to let the liquid on the sieve run through. Change the liquid in the dish after every two brushing periods. Continue this operation until the wash liquid passing over the residue and through the sieve is clear and free from solid particles. When the washing appears to be complete, collect about 200 mL of the wash liquid, after passing over the residue and through the sieve, in a clean 400-mL beaker. Stir the liquid vigorously, and set the beaker on a black surface in the case of white pigments and on a white surface in the case of colored pigments. The washing is not considered complete until such a test fails to show any particles collected about the middle of the bottom of the beaker. Nyz' 1--Occasionally, pigments will be found that foam when water is used as the wash liquid. In such instances, during the last washing in the porcelain dish the use of a liquid that breaks down the foaming and is readily miscible with water, such as alcohol, will usually overcome this difficulty. 5.5 When the washing is complete wash the pigment particles adhering to the brush back onto the sieve and wipe off the water below the sieve. Add a few drops of alcohol and then of ether to expedite drying. Dry the sieve for 1 h at ! i j 1 1 j | f f i j f j j * | I j ' 105" perc 6. P 6. folio the i of w 7. P 7. 7.: usinj with, filter be si 7.: mate moti a tir parti heav carb. into throi 7.` throi same gone most Add agen wate tion abou poin persi the f easil; each centi man to re blacl 7.; weigl the v as fc throi the s carbe black to th coars 24 DUP050297207 1 mg. i basic ie, 2g ussian of the >. Wet :r the 1. to 500 taking A soft ion. If gment rocess, ipidly, gment ling to D-mm) so that sh the 5-mm) second ne dish e run 1 two wash s clear ars to , after . clean beaker d on a shing is ow any of the ien water ishing in ning and :ome this ligment ad wipe hoi and 1 h at D 185 105C, cool, and weigh as described in 5.1. Calculate the percent of coarse particles. 6. Procedure foT Metallic Aluminum and Bronze Powders 6.1 In the case of metallic aluminum and bronze powders follow the procedure described in Section 5 except use 5 g of the material as the specimen and denatured alcohol, instead of water, as the wash liquid. 7. Procedure for Carbon Black in Pellet Form 7.1 Dry, cool, and weigh the sieve as described in 5.1. 7.2 Prepare a stock solution of dispersing agent3 in water; using as high a concentration of dispersing agent as possible without losing fluidity. When solution has been obtained, filter through coarse filter paper. A quart of this solution will be sufficient for several tests. 7.3 Crush the pellets between two glass plates approxi mately 12-in. (305-mm) square, using a gentle rotating motion. If 10 g of carbon black are taken, crush about 2 g at a time. Weigh into a 600-mL beaker 10 g of the crushed particles. Add enough of the dispersing solution to make a heavy paste and mix well to incorporate thoroughly the carbon black. Dilute with water to about 300 mL; then pour into the clean 45-pm (No. 325) sieve. First pass the tap water through a 45-pm sieve. 7.4 Using a small camel's-hair brush, gently brush the mix through the sieve, running tap water slowly through at the same time. When it appears that all the dispersed black has gone through, stop the tap water and continue brushing until most of the water remaining on the sieve has gone through. Add a few millilitres of the stock solution of the dispersing agent, thoroughly mix with the brush, then turn on the tap water again and wash through as before. Repeat this opera tion until no dispersed black comes through the sieve. When about 0.5 g of sand-like material is left on the sieve, the end point is being approached. At this point, adding the dis persing solution and gently rubbing it into the residue with the finger still produces a colloidal dispersion of black which easily passes through the sieve. From this point on, before each addition of dispersing agent, work the residue into the center of the sieve with the tap water. Many washings and many additions of dispersing solution are required in order to reach the end point. Take care to make certain that all the black has been washed through the sieve. 7.5 Dry the sieve in an oven at 105C for 1 h, cool, and weigh the residue. Calculate the percent of coarse particles. If the value thus obtained is greater than that specified, proceed as follows to remove any adhered carbon that will pass through the 45-pm (No. 325) sieve; Transfer the particles on the sieve to a piece of white bond paper and gently rub the carbon onto the paper with the finger. When no further real blackening of the paper occurs, carefully transfer the residue to the balance pan, weigh, and recalculate the percent of coarse particles. 8. Procedure for Water-Soluble Pigments, Pastes in Oil, Pastes in Japan, and Mixed Paints 8.1 Dry, cool, and weigh the sieve as described in 5.1. 3 Any dispersing agent specific for carbon black may be used, such as Damn No. 1 available from R.T. Vanderbilt, 30 Winfield St., Norwalk, CT 06S55. 8.2 For water-soluble pigments use 10 l g as the specimen. For pastes in oil, pastes in Japan, and mixed paints use 25 I g as the specimen. For white leads and red lead use 50 1 g as the specimen. 8.3 Weigh the specimen to 1 mg and transfer to a 250-mL beaker. Slowly add 100 mL of kerosine to the contents of the beaker, mixing thoroughly by use of a stirring rod with flattened end. Break up all lumps but do not grind the material. 8.4 Wet the sieve on both sides with kerosine; then transfer the contents of the beaker to the sieve using a wash bottle filled with kerosine. 8.5 Remove small particles retained on the stirring rod or beaker walls with a camel's-hair brush. Rinse the brush with kerosine. 8.6 When the washing is complete, wash the pigment particles adhering to the brush back onto the sieve and wipe off kerosine below the sieve. Dry the sieve for 1 h at 105C, cool, and weigh as described in 5.1. Calculate the percent of particles. 9. Procedure for Ship-Bottom Paints Containing Resins and Alcohol 9.1 In the case of ship-bottom paints containing resins and alcohol follow the procedure described in Section 8, with specimen weight of 25 1 g, but use denatured alcohol, instead of kerosine, as the wetting medium, for mixing with paint, and as the wash liquid. 10. Procedure for Cellulose Ester Lacquers 10.1 In the case of cellulose ester lacquers follow the procedure described in Section 8, with specimen weight of 25 1 g of the material but use a mixture ofequal parts of ethyl acetate, toluene, and denatured alcohol, instead of kerosine, as the wetting medium, for mixing with the lacquer, and as the wash liquid. 11. Procedure for Latex and Emulsion Paints 11.1 Apparatus--As described b Section 4 except that sieves used shall be as follows: 11.1.1 Flat Paints, a 3-in. (75-mm) 90-pm (No. 170) sieve. 11.1.2 Gloss and Semi-Gloss Paints, a 3-in. (75-mm) 75-pm (No. 200) sieve. 11.2 Dry, cool, and weigh the sieve as described in 5.1. 11.3 Weigh 25 g of paint to 1 g into a tared 250-mL beaker. Without delay, start adding 100 mL of water to the paint in the beaker, slowly and with hand stirring sufficient to thoroughly mix the paint with the water. Wet the sieve on both sides with water and transfer the contents of the beaker gradually to the sieve, using a wash bottle containing water. Small particles retained on the stirrer or beaker walls may be removed with a camel's-hair brush. Instead of tap water, use reagent water for diluting the paint sample, in the wash bottle, and for washing the paint through the sieve. The water may be delivered from a reservoir for the last step. 11.4 Follow the procedure described in 5.3. In using the camel's-hair brush, take care not to crush agglomerates that would not be broken down in normal application of the paint. Rinse the brush into the sieve at end of use. 11.5 Finally, dry, cool, and weigh the sieve for l h, as DUP0502 97208 do 185 described in 5.1. Then calculate the percent of coarse particles and skins. 12. Precision 12.1 Precision data are not available at this time. When available the appropriate precision statements will be added. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years end if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. i 1. wl T pr. re: ap ap 2. | '1 1 I I I ! 1 f. I I r E E # Rela- DOI. C publi I 26 DUP0502 97209 Designation: D 215 - 91 Standard Practice for the Chemical Analysis of White Linseed Oil Paints1 This standard is issued under the fixed designation D 215; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice covers the chemical analysis of the usual white linseed oil paints. The methods included are listed in Table 1. 1.2 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsibiliity of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D34 Practice for Chemical Analysis of White Pigments2 D 50 Methods of Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese2 D 280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pig ments2 D717 Test Methods for Analysis of Magnesium Silicate Pigment2 D1193 Specification for Reagent Water3 D1208 Test Methods for Common Properties of Certain Pigments2 D1301 Test Methods for Chemical Analysis of White Lead Pigments2 D1394 Test Methods for Chemical Analysis of White Titanium Pigments2 D1398 Test Method for Fatty Acid Content of Alkyd Resins and Alkyd Resin Solutions2 D1469 Test Methods for Total Rosin Acids Content of Coating Vehicles2 D1542 Test Method for Qualitative Detection of Rosin in Varnishes4,5 D 1959 Test Method for Iodine Value of Drying Oils and Fatty Adds4 D 2349 Method of Qualitative Determination of Nature of Thinner in Solvent-Redudble Paints5 D2350 Test Method for Antimony Oxide in White Pigment Separated from Solvent-Redudble Paints2 D2351 Test Method for Sulfide in White Pigment Sepa rated from Solvent-Redudble Paints2 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO1.2 3 on Chemical Analysis of Paint and Paint Materials. Current edition approved May 15, 1991. Published July 1991. Originally published as D 215 -25 T. Last previous edition D215-73 (1979). 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vol 06.01. D2352 Test Method for Sulfur Dioxide in White Pigment Separated from Solvent-Reducible Paints2 D2369 Test Method for Volatile Content of Coatings5 D2371 Test Method for Pigment Content of Solvent- Reducible Paints5 D2372 Method of Separation of Vehicle from Solvent- Reducible Paints5 3. Purity of Reagents 3.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 3.2 Unless otherwise indicated, references to water shall be understood to mean Type II reagent grade water con forming to Specification D 1193. 4. Hazards 4.1 Ammonium Hydroxide causes severe burns and may be fetal if swallowed. Read the appropriate Material Safety Data Sheets (MSDS) before using. 4.2 Hydrochloric and Sulfuric Acids cause severe bums and may be fatal if swallowed. Read the appropriate MSDS before using. 4.3 Acetic Acid causes severe bums and may be fatal if swallowed. Read the appropriate MSDS before using. 4.4 Nitric Acid causes bums and may be fetal if swal lowed. Vapor is extremely hazardous and may cause ni trogen oxide poisoning. Read the appropriate MSDS before using. 4.5 Toluene is flammable. Vapors are harmful. Use with adequate ventilation. Read the appropriate MSDS before using. 4.6 Hydrogen Sulfide is both an irritant and an asphyxiant. Read the appropriate MSDS before using. 4.7 Ammonium Sulfide evolves hydrogen sulfide on con tact with acid or acid fumes. See 4.6. Read the appropriate MSDS before using. 4.8 Barium Chloride--Soluble barium salts are poisonous when taken by mouth. Read the appropriate MSDS before using. `"Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc., Washington. D.C. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nosttand Co., inc.. New York, N. Y., and the "United States Pharmacopeia." 27 DUP050297210 D 215 TABLE 1 List of Test Methods Test Method Preparation of Sample Water Volatile Thinner Nature of Thinner Percentage of Pigment Percentage of Nonvolatile Vehicle Separation of Vehicle Unsaponifiable Matter Fatty Acids Iodine Number of Fatty Acids Resin Qualitative Analysis. Single. Mixed, or Composite Pigments Quantitative Analysis, Single Pigment Quantitative Analysis, Mixed or Composite Pig ments: Moisture and Other Volatile Matter Loss on Ignition Insoluble Matter Total Lead (Antimony) Antimony Oxide Soluble Barium Aluminum Oxide Total Zinc Soluble Calcium Soluble Magnesium Carbon Dioxide Total Soluble Sulfur Compounds Soluble Sulfate Sulfide Sulfur Sulfur Dioxide Matter Soluble in Water Section 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 ASTM Method D1208 D 2369 D2349 02371 D 2372 D1397 D1398 01959 D1542 D34 D 280 D1208 ... D 2350 D1301 034 D50 D2351 02352 01208 5. Preparation of Sample 5.1 On receipt of a sample, make a record of the label noting espedaily the brand, the name of the manufacturer, and any statement as to the composition of the paint and the net contents. Weigh the unbroken package, open, note odor and condition of the contents, pour into a clean container, and mix thoroughly by pouring from one container to the other, finally leaving the well-mixed sample in the second container which shall be tightly closed. The well-mixed sample shall be used at once for the analysis. The original can and cover may be cleaned with a suitable solvent, wiped dry, and then weighed. This weight subtracted from the original weight will give the net weight of the contents. If desired, the specific gravity of the paint may be determined, the weight per gallon calculated, and the volume ofpaint and the capacity of the container may be measured. ANALYSIS OF PAINT 6. Water 6.1 Determine water in accordance with Test Methods D 1208. 7. Volatile Thinner 7.1 Determine the volatile matter in accordance with Test Method D 2369. Calculate the loss in weight as the per centage of water and volatile thinner. Subtract from this the percentage of water as determined in accordance with Section 6. Report the remainder as percent volatile thinner. 8. Nature of Thinner 8.1 Determine the nature of the thinner in accordance with Method D 2349. 9. Percentage of Pigment 9.1 Determine the percentage of pigment in accordance with Test Method D 2371. Preserve the pigment as prepared in a stoppered bottle for use in Sections 16 and 17. 16 cono tion- 16. 10. Percentage of Nonvolatile Vehicle 10.1 Add together the percentages of water, volatile thinner, and pigment, and subtract the sum from 1Q0. Report the remainder as nonvolatile vehicle. 16. 16. 16. Disso 3H20 TESTING NONVOLATILE VEHICLE 11. Separation of Vehicle j f J 11.1 Separate the vehicle from the pigment in accordance 1 with Method D 2372. Retain the vehicle so obtained for use ] in the unsaponifiable matter (see 12.1) and fatty acids (see 13.1) determinations. about freshl: in 10 small alkalij gr 1.1' nearly 12. Unsaponifiable Matter 12.1 Determine the unsaponifiable content of the vehicle in accordance with Test Method D 1398. from a a whit shows run wi 13. Fatty Acids f 13.1 Determine the fatty acids in accordance with Method ! D 1398. standa: quired used ir standai 14. Iodine Number of Fatty Acids 14.1 Determine the iodine number of fatty acids (see temper sample 16.1. 13.1) in accordance with Test Method D 1959. 16.1. N{|' 1 --Ifappreciable amounts of rosin or of unsaponifiable matter I are found to be absent in the vehicle ofa paint, the iodine number ofthe j fatty acids gives the best indication (though not proof) of the presence of 1 linseed oil. An iodine number of less than 175 (Wijs) for the fatty acids f is an indication that the nonvolatile vehicle was not pure linseed oil. | 15. Rosin I 15.1 Determine the presence of rosin in the fatty acids 1 (see 13.1) in accordance with Test Method D 1542. | 15.2 If desired, determine the amount of roan quantiia-| tively in accordance with Method D 1469. 1 acid (H 16.1. concent 19 volu 16.2 16.2.1 and the acetic a decompt large exc and tesi ANALYSIS OF PIGMENT | (especiai Qualitative Analysis, Total Pigments--Single, Mixed, srl Composite I this filtr; calcium absence 16. Qualitative Analysis 16.1 Reagents: contain : I N}~' 2 16.1.1 Acetic Acid. (Precaution--See 4.3) 16.1.2 Acid Ammonium Acetate Solution--Mix 150 mlol acetic acid (8+2) 100 ml of water, and 95 ml of NH4OH (sp gr 0.90). 16.1.3 Ammonium Hydroxide (spgr 0.90)--Concentrate] ammonium hydroxide (NH4OH). (Precaution--See 4.1) some st as calcii not bee calcium 16.1.4 Ammonium Polysulfide--Pass H2S gas into 200 i of NH4OH (sp gr 0.90) in a bottle immersed in runniS water or in iced water until the gas is no longer abso then add 200 mL of NH4OH (sp gr 0.90) and dilute water to 1 litre. Digest this solution with 25 g of flowers 16.2. acetate finally 'gnited, sulfur for several hours and filter. 16.1.5 Ammonium Sulfate ((NH4)2S04). 16.1.6 Barium Chloride (BaCl2 2H20). (Precaution 4.8) 28 DUP050297211 :cordance prepared , volatile rom 100. ccordance ed for use acids (see he vehicle th Method acids (see liable matter umber of the e presence of ie fatty acids inseed oil. ; i j j ! 1 fatty acids 12. a quantita- Mixed, or x150 ml of i NH4OH (sp I oncentrated See 4.1) into 200 ml in running ;r absorbed; dilute with )f flowers of j | taution--See D 215 16.1.7 Hydrochloric Acid (1+1)--Mix equal volumes of concentrated hydrochloric acid (HCl, sp gr 1.19) (Precau tion--See 4.2) and water. 16.1.8 Hydrogen Peroxide (H202), 3%. 16.1.9 Hydrogen Sulfide (HUS). (Precaution--See 4.6) 16.1.10 Potassium Dichromate (K2Cr207). 16.1.11 Potassium Ferrocyanide, Standard Solution-- Dissolve 22 g of pure potassium ferrocyanide (K4Fe(CN)6 3H20) in water and dilute to 1 L. To standardize, transfer about 0.2 g (accurately weighed) of pure metallic zinc or freshly ignited pure zinc oxide to a 400-mL beaker. Dissolve in 10 mL of HCl (sp gr 1.19) and 20 ml of water. Drop in a small piece of litmus paper, add NH4OH until slightly alkaline, add HCl until just acid, and then 3 mL of HCl (sp gr 1.19), Dilute to about 250 mL with hot water and heat nearly to boiling. Run in the K4Fe(CN)6 solution slowly from a buret, while stirring constantly, until a drop tested on a white porcelain plate with a drop of the uranyl indicator shows a brown tinge after standing 1 min. A blank should be run with the same amounts of reagents and water as in the standardization. The amount of JCtFefCNJfi solution re quired for the blank should be subtracted from the amounts used in standardization and in titration of the sample. The standardization must be made under the same conditions of temperature, volume, and acidity as obtained when the sample is titrated. 16.1.12 Potassium Iodide (KI). 16.1.13 Sulfuric Acid {sp gr 1.84)--Concentrated sulfuric acid (H2S04). (Precaution--See 4.2) 16.1.14 Sulfuric Acid (1+19)--Carefully mix 1 volume of concentrated H2S04 (sp gr 1.84) (Precaution--See 4.2) with 19 volumes of water. 16.2 Procedure: 16.2.1 The following qualitative analysis should be made and the quantitative scheme modified as required Add acetic acid slowly to the pigment until all carbonate is decomposed (noting whether any H2S is evolved), then add a large excess of acid ammonium acetate solution. Boil, filter, and test the filtrate for metals other than lead and zinc (especially calcium and barium). The absence of calcium in this filtrate indicates that the extending pigments contain no calcium carbonate (CaC03) or calcium sulfate (CaS04); the absence of barium indicates that the extending pigments contain no barium carbonate (BaC03). N' 2--If the original sample contained BaC03, and lead sulfate (PbS04), CaS04, or other soluble sulfate, the soluble barium will form with the soluble sulfate a precipitate of BaS04 which will be determined as "insoluble matter." If the sample contained strontium sulfate (SrS04) or strontium carbonate (SrC03), some SrS04 may be counted as BaS04, some strontium will count as soluble barium, and some may be counted as calcium oxide (CaO). Strontium is not separated, as it probably will not be encountered, or will be present as an impurity in the barium and calcium compounds. 16.2.2 Wash the matter insoluble in acid ammonium acetate solution with another portion of this solution, and finally with hot water. This insoluble matter shall be dried, ignited, and tested for siliceous matter, BaS04, and titanium compounds. To test for the latter, place a small amount of the insoluble matter, or of the original sample (about 0.5 g) in a 250-mL resistant glass beaker; add 20 mL of concen trated H2S04 (sp gr 1.84) and 7 to 8 g of (NH4)2S04. Mix well, and boil for a few minutes. A residue denotes the presence of silica or siliceous matter. Cool the solution, dilute with 100 mL ofwater, heat to boiling, settle, filter, and wash with hot H2S04 (1 + 19) until free from titanium. The residue may be tested for lead, barium, and silica. 16.2.3 Add H202 to a small portion of the filtrate; a clear yellow-orange color indicates the presence of titanium. Boil another portion of the filtrate with metallic tin or zinc; a pale blue to violet coloration indicates titanium. 16.2.4 Treat another portion (about 1 g) of the pigment with 20 ml of HCl (1+1) and note whether any H2S is evolved; boil the solution for about 5 min, add about 25 ml of hot water, filter, and wash with hot water. Render a small portion of the filtrate alkaline with NH4OH, acidify with HCl, and add a little BaCl2 solution; a white precipitate (BaSO,,) indicates the presence of a soluble sulfate. To another portion of the filtrate add a little H2S04; a white precipitate indicates the presence of lead, soluble barium, or both (some CaS04 may also separate). Filter, wash to remove free acid, and treat the precipitate with a few drops of KI solution; the formation of yellow lead iodide (Pbl2) indicates the presence of lead. The white precipitate may also be treated with H2S water, the formation of black lead sulfide (PbS) indicates the presence of lead. 16.2.5 To another portion of the original filtrate (see 16.2.1) add NH4OH until alkaline, render slightly acid with acetic acid, heat to boiling, and add a little K2Cr207 solution; a yellow or orange-yellow precipitate indicates the presence of lead, soluble barium, or both. To another portion of the original filtrate add a few drops of IQFetCNjg solution; a white precipitate with a bluish tinge indicates the presence of zinc. Pass into the remaining portion of the original filtrate a current of H2S for 5 to 10 min, add an equal volume of water, and pass H2S into the solution for about 5 min. Filter and wash with H2S water. Digest the precipitate with ammonium polysulfide, filter, acidify the filtrate with HCl, and warm; the presence of antimony is indicated by the separation ofan orange-colored precipitate. The filtrate from the H2S precipitate may be tested for barium, calcium, and magnesium in the usual manner. Quantitative Analysis, Single Pigment 17. Quantitative Analysis 17.1 If the sample is a single pigment, proceed in accord ance with Practice D34, for the particular pigment to be tested. Quantitative Analysis, Mixed or Composite Pigments 18. Moisture and Other Volatile Matter N ' 3--On an extracted and dried pigment, this determination is of little value. If the original paint contained gypsum, a part of the combined water of the latter will be driven off in the drying of the extracted pigment and in the "moisture" determination. 18.1 Determine the moisture and other volatile matter in accordance with Test Methods D 280. 19. Loss on Ignition N ' 4--This determination may serve as a rough or approximate check in many cases on the carbon dioxide, water, etc. 19.1 Determine loss on ignition in accordance with Test Methods D 1208. 29 DUP050297212 215 20. Insoluble Matter 20.1 Reagents: 20.1.1 Alcohol 20.1.2 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric acid (HC1). (Precaution--See 4.2) 20.1.3 Hydrochloric Acid (1+1)--Mix equal volumes of concentrated HC1 (sp gr 1.19) (Precaution--See 4.2) and water. 20.1.4 Sodium Carbonate (Na2C01), anhydrous. 20.1.3 Sodium Carbonate (10 g/L)--Mix 10 g of Ma2C03 with water and dilute to 1 L. 20.1.6 Sulfuric Acid (1+4)--Carefully mix 1 volume of concentrated sulfuric acid (H2S04, sp gr 1.84) (Precaution-- See 4.2) with 4 volumes of water. 20.2 Procedure: 20.2.1 Moisten 1 g of the pigment with a few drops of alcohol, cover, add 40 ml of HCI (1+1) and boil gently for 5 to 10 min. Wash the cover, evaporate to dryness, and heat at about 150C for 30 min to 1 h to dehydrate the residue. Moisten the residue with 4 ml of concentrated HCI (sp gr 1.19), allow to stand a few minutes, dilute with 100 ml of hot water, boil a few minutes, filter hot through paper, and wash with hot water (until washings give no test for lead and chlorine). 20.2.2 Ignite the paper and residue in a platinum or porcelain crucible, cool, and weigh the total insoluble matter (Note 2). (The insoluble matter may be filtered off on a Gooch crucible, washed with hot water, dried at 105"C, cooled, and weighed; it shall then be ignited, cooled, and weighed, when it is desired to get the loss on ignition (combined water, organic matter, etc.) of the same, or if the insoluble matter is not to be further examined.) If the sample contains titanium pigment, practically all of the titanium dioxide (1102) will be found in the insoluble matter along with barium sulfate (BaS04) and siliceous matter. Should an examination of the insoluble matter be necessary, it is advisable to remove the Ti02 before proceeding further. The TiOj may be remove'1 (or determined on a separate portion) in accordance with t Methods D 1394. 20.2.3 After removing the Ti02, the residue containing siliceous matter and BaS04 may be ignited to remove the filter. To determine BaS04, mix the ignited insoluble matter with about ten times its weight of anhydrous Na2C03 (grinding the mixture in an agate mortar if necessary) and fuse in a covered platinum crucible, heating about 1 It Let cool, place the crucible and the cover in a 200-mL glazed porcelain casserole (Note 5), add about 100 mL ofwater, and heat until the mass is disintegrated. Filter on paper into a 300-mL glazed porcelain casserole (leaving the crucible and the cover in the original casserole) and wash the casserole and filter thoroughly with a hot solution ofNa2C03 (10 g/L). Place the casserole containing the crucible and cover under the funnel, pierce the filter with a glass rod, and wash the residue into the original casserole by means of a jet of hot water. Wash the paper with hot HCI (1 +1) and then with hot water. Remove the crucible and the cover. Evaporate the HCI solution to dryness, and heat at about 150C for 30 min to 1 h. Moisten the residue with about 10 mL of concen trated HCI (sp gr 1.19), dilute with 100 mL of hot water, boil a few minutes, filter hot through paper, and wash thoroughly with hot water. Dilute the filtrate to a volume of 300 mL, bring to boiling, and add, dropwise, 5 mL of H2S04 (1+4) Allow to stand in a warm place for 1 h or so, filter on a weighed Gooch crucible, wash with hot water, ignite, cool and weigh as BaS04. Subtract the sum of the percentage 0f BaS04 and Ti02 from the percentage of total insoluble matter and report the result as the percentage of insoluble siliceous matter (Note 6). N' 5--A casserole is preferable to a beaker, as silica is dissolved from glass when in long contact with a strong sodium carbonate solution. No t e 6--Any soluble aluminum oxide (A1203) (or iron oxide (Fe^)) and in most cases magnesium oxide (MgO), and sometimes some calcium oxide (CaO), come from the siliceous pigment used Magnesium oxide generally denotes the presence of asbestine. 20.2.4 To determine silica, acidify the filtrate from the barium carbonate (BaC03) filtration (20.2.3) with HCI, boil to expel the COz, evaporate to dryness, bake to dehydrate the silica, moisten with HCI, dilute with 100 mL of hot water, and boil and filter through the same paper as was used to recover silica from the BaC03 portion. Wash thoroughly with hot water and proceed in accordance with Test Methods D717. 20.2.5 If it is desired to look for magnesium, combine the filtrate obtained in accordance with 20.2.4 with the filtrate from the final BaS04 separation (20.2.3) and test for A1203 and MgO in the usual way. To recover MgO that may have dissolved in the procedure for the elimination of the Ti02, make the* filtrate containing the Ti02 just alkaline with NH4OH, bring to boiling, filter, and wash. The filtrate may be tested for MgO. Any A1203 present will be precipitated along with the Ti02. To recover this, ignite and weigh as Ti02 and A1203. Deduct for Ti02 present in the sample; the difference is A1203. 21. Total Lead 21.1 Reagents: 21.1.1 Acetic Acid: Precaution--See 4.3. 21.1.2 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). Precaution--See 4.1. 21.1.3 Ammonium Polysulfide--See 16.1.4; 21.1.4 Ammonium Sulfide ((NH4)2S). Precaution--See 4.7. 21.1.5 Ether. 21.1.6 Ethyl Alcohol (95%). 21.1.7 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric acid (HCI) Precaution--See 4.2. 21.1.8 Hydrogen Sulfide (H2S). Precaution--See 4.6, 21.1.9 " LeadAcid"--Mix 300 ml of concentrated H2S04 (sp gr 1.84) and 1800 ml of water. Dissolve 1 g of lead acetate in 300 mL of water and add this to the hot solution while stirring. Let stand at least 24 h and siphon through a thick asbestos filter. 21.1.10 Nitric Acid (1+1)--Mix equal volumes of concen trated nitric acid (HN03, sp gr 1.19) (Precaution--See 4.4) and water. 21.1.11 NitricAcid (1+3)--Mix 1 volume ofconcentrated HN03 (sp gr 1.19) (Precaution--See 4.4) with 3 volumes of water. 21.1.12 Potassium Dichromate Solution (100 g/L)--Dis solve 100 g ofpotassium dichromate (K2Cr207) in water and dilute to 1 L. 30 21 20 tc L. 21. add 1 21. conct 1 vol 21. 21. to 20' pass 1 volun with (1+3) H2SO evolvt mL o crudt 105 tc and w (PbO) No t carbon, metals, nor bas 21.2 the si precip porcel polysu 60C 1 cover, to 30 the res lead si sulfide on a se sampli boil ge to dry dissoh amour HCI (s minuti until t contair 21.2. evapor; copious then ad Heat ti comple settle 01 tempers Quickly solution asbestos DUP050297213 1+4). on a cool, ges of Muble }luble ssolved bonate oxide letimes t used. n the 1, boil ite the water, sed to Highly ;thods ne the lltrate A1203 / have Ti02, : with e may ritated igh as le; the itrated L. --See d hy- 6. H2S04 acetate , while l thick oncenee 4.4) itrated mes of --Dister and D 215 21.1.13 Sodium Sulfide Solution (20 to 30 g/L)--Dissolve 20 to 30 g of sodium sulfide (Na2S) in water and dilute to 1 L. 21.1.14 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid (H2S04). Precaution--See 4.2. 21.1.15 Sulfuric Acid (1+1)--Carefully mix 1 volume of concentrated H2S04 (sp gr 1.84) (Precaution--See 4.2) with 1 volume of water. 21.2 Procedure: 21.2.1 Unite the filtrate and washings (total volume 150 to 200 mL) from the total insoluble matter (see Section 20), pass H2S into the solution until it is saturated, add an equal volume of water, and again saturate with H2S. Filter, wash with water containing a little H2S, dissolve in hot HN03 (1+3), washing the paper with hot water. Add 10 to 20 mL of H2S04 (1+1), evaporate until copious fumes of H2S04 are evolved. Cool, add about 75 ml of water and then about 75 mL of ethyl alcohol (95%). Stir, let settle, filter on a Gooch crucible, wash with diluted alcohol, and dry in an oven at 105 to 110'C; or, ignite gently in a radiator7 or muffle, cool, and weigh as lead sulfate (PbS04). Calculate to lead oxide (PbO). N' 7--It is not possible to determine the amount of basic lead carbonate and lead sulfate when carbonates or soluble sulfates of other metals, such as calcium, are present. Also, neither basic lead carbonate nor basic lead sulfate are definite compounds. 21.2.2 If the pigment contains antimony, filter and wash the sulfide precipitate as described in 21.2.1. Wash the precipitate with a fine jet of water from the paper into a porcelain dish or casserole, add 25 mL of ammonium polysulfide, cover the vessel, and warm the mixture at 40 to 60C for 10 to 15 min while stirring frequently. Wash the cover, filter through the same paper, and wash with Na2S (20 to 30 g/L) or (NH4)2S solution. Discard the filtrate. Dissolve the residue in hot HN03 (1+3), and determine the lead as lead sulfate (PbS04) as described in 20.2.1; or, the original sulfide precipitate may be discarded and the lead determined on a separate portion of the pigment as follows: to 1 g of the sample in a covered beaker, add 40 mL of HC1 (1+1) and boil gently for 5 to 10 min. Wash off the cover and evaporate to dryness. To the residue add sufficient HC1 (sp gr 1.19) to dissolve the PbS04 (with pigments containing considerable amounts of PbS04, it may be necessary to add 15 to 20 ml of HC1 (sp gr 1.19)), add about 50 mL of hot water, boil a few minutes, filter hot through paper, and wash with hot water until the washings give no test for lead. (If the sample contains no insoluble matter, omit the filtration.) 21.2.3 To the filtrate add 20 mL of H2S04 (sp gr 1.84) and evaporate until dense white fumes of sulfur trioxide (S03) are copiously evolved. Allow to cool, but not below 60C, and then add slowly 50 mL of water while agitating the solution. Heat to boiling for several minutes in order to ensure complete solution of antimony sulfate. Allow the PbS04 to settle out until the supernatant liquid is clear, not letting the temperature fall below 60C. If the liquid does not clear quickly it must be heated longer. When clear, pour the solution through a weighed porcelain Gooch crucible with asbestos mat, decanting the solution as completely as pos-1 1 U. S. Geological Survey. Bulletin 700 (1919), p. 33. sible without allowing more than a very small amount of PbS04 to go over into the crucible. Add 10 mL more of concentrated H2S04 (sp gr 1.84) to the PbS04 in the original beaker and boil for several minutes. Cool, add slowly 30 mL of water, and again heat to boiling for a few minutes. Allow the solution to cool to about 60"C and completely transfer the PbS04 to the Gooch crucible. Wash with "lead acid" (see 21.1.9) to remove soluble sulfates and finally wash free of acid with diluted alcohol (equal parts of ethyl alcohol or denatured alcohol and water). Dry in an oven at 105 to 1 ICC, or ignite gently in a radiator or muffle. Calculate to PbO, or determine as lead chromate (PbCr04) as described in 21.2.6. 21.2.4 If soluble compounds of barium or calcium are present, barium sulfate (BaS04) and calcium sulfate (CaS04) will be included with the PbS04. If soluble silica (Si02) is present, it will also be included with the PbS04. In such cases, the PbS04 precipitate after washing with diluted alcohol may be dissolved in acid ammonium acetate and the lead determined as PbCr04 as described in 21.2.6. For ordinary work, the amount of BaS04 dissolved by the acetate treatment may be disregarded. 21.2.5 If the pigment contains no soluble antimony, barium, or calcium compounds, the lead may be determined directly on the original pigment as follows: to 1 g of the sample in a covered beaker, add 25 mL of HN03 (1+1) and boil gently a few minutes. Wash off the cover, evaporate to dryness on a steam bath, moisten with HN03, add hot water, and heat a few minutes. Filter and wash with hot water until washings are lead-free. Add 10 to 20 ml of H2S04 (1+1) to the clear solution, evaporate, and determine lead as PbS04 as described in 21.2.1. 21.2.6 In the absence of soluble compounds of antimony, iron, aluminum, and barium, the following procedure may be used: treat 1 g of the original pigment with 25 mL of HN03 (1+1) and proceed as described in 20.2.1. To the clear solution, diluted to 200 mL, add NH4OH in slight excess, acidify with acetic acid, and add 4 to 6 mL more of acetic acid. Heat to boiling and add 10 to 15 mL of a solution of K2Cr207 (100 g/L). Heat until the yellow precipitate assumes an orange color, let settle, and filter on a weighed Gooch crucible. Wash by decantation until the washings are color less, finally transferring all of the precipitate. Wash with ethyl alcohol (95 %) and then with ether. Dry to constant weight at 110C, cool, and weigh as PbCr04. Calculate to PbO. 22. Antimony Oxide 22.1 Determine antimony oxide in accordance with Test Method D 2350. 23. Soluble Barium 23.1 Boil the combined filtrate and washings, reduced to volume by evaporation if need be, from the lead sulfate (PbS) precipitate (see 21.2) to expel hydrogen sulfide (H2S). Add a slight excess of H2S04 (1+4) over the amount required to precipitate the barium, heat to boiling, let stand on a steam bath about 1 h, filter on a weighed Gooch crucible, wash with hot water, dry, ignite, cool, and weigh as barium sulfate (BaS04) (Notes 2 and 8). Calculate to barium oxide (BaO). N' 8--The precipitate will include any BaS04 that may have been dissolved as such. The weighed precipitate should be tested for CaS04, 31 DUP050297214 D 215 and if present, it should be removed by treating with hot HQ (1+3), filtering, washing, igniting, and again weighing. 24. Aluminum Oxide (Fe302, Ti02, P205) 24.1 Reagents: 24.1.1 Ammonium Chloride Solution (25 g/L)--Dissolve at least 25 g of ammonium chloride (NH4C1) in water and dilute to 1 L. 24.1.2 Ammonium Hydroxide (/+5)--Mix 1 volume of concentrated ammonium hydroxide (NH4OH, sp gr 0.90) (Precaution--See 4.1) with l volume of water. 24.1.3 Hydrochloric Acid {sp gr 1.19)--Concentrated hy drochloric acid (HC1). Precaution--See 4.2. 24.1.4 Methyl Red Indicator, Alcoholic Solution (2 g/ L)--Dissolve 0.2 g of methyl red in alcohol and dilute to 100 mL. 24.1.5 Nitric Add (sp gr 1.42)--Concentrated nitric acid (HN03). Precaution--See 4.4. 24.2 Procedure; 24.2.1 Boil the filtrate from the lead sulfide (FbS) precip itate (see 21.2) to expel hydrogen sulfide (H2S), add a few drops of HN03, and continue the boiling a few minutes to oxidize any iron that may be present. In case soluble barium was present, use the filtrate from 23.1. To the solution containing at least 25 g of NH4CI/L of solution, or an equivalent amount of HC1, add a few drops of methyl red indicator, alcoholic solution and heat just to boiling. Care fully add NH4OH (1+5) dropwise until the color of the solution changes to a distinct yellow. Boil the solution for I to 2 min and filter at once. Wash the precipitate thoroughly with hot NH4CI solution (Note 9). Ignite the precipitate, cool, and weigh as aluminum oxide (A1203) (Note 10). No t e 9--For very accurate work, or when the precipitate is large, the precipitate should be dissolved in HC1 (1+1) and the precipitation repeated. No t e 10--This precipitate may also contain ferric oxide (Fe203), titanium dioxide (Ti02), and phosphorus pentoxide (P2Os). 25. Total Zinc 25.1 Reagents: 25.1.1 Acetic Acid (14-49)--Mix I volume of concen trated acetic acid (sp gr 1.05) (Precaution--see 4.3) with 49 volumes of water. 25.1.2 Ammonium Acetate. 25.1.3 Ammonium Chloride (NH4C1). 25.1.4 Ammonium Hydroxide (sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). Precaution--See 4.1, 25.1.5 Hydrochloric Acid (sp gr 1.19)--Concentrated hy drochloric acid (HC1) Precaution--See 4.2. 25.1.6 Hydrochloric Acid (1+2)--Mix 1 volume of con centrated HC1 (sp gr 1.19) (Precaution--See 4.2) with 2 volumes of water. 25.1.7 Hydrogen Sulfide (H2S). Precaution--See 4.6. 25.1.8 Potassium Ferrocyanide, Standard Solution--See 16.1.11. 25.1.9 Uranyl Indicator--Dissolve 5 g of uranyl nitrate in water and dilute to 100 mL, or dissolve 5 g of uranyl acetate in water made slightly acid with acetic acid and dilute to 100 mL. 25.2 Procedure: 25.2.1 To the combined filtrate and washings from the alumina determination (see 24.2.1), add sufficient NH4C1 to 32 DUP050297215 Dilute the clear filtrate to about 200 mL with water, add 30 mL of HC1 (1+2), and a small piece of litmus paper; add NH4OH (sp gr 0.90) until slightly alkaline, render just add with HC1, then add 3 mL of concentrated HCI (sp gr 1.19), heat nearly to boiling, and titrate with K^FefCN)^ solution as described in 25.2.4. Calculate this result to zinc, subtract from total zinc, and calculate the difference to zinc sulfide (ZnS). (Any zinc carbonate (ZnC03) or zinc sulfate (ZnS04) is included in the ZnO.) 26. Soluble Calcium 26.1 Reagents: 26.1.1 Ammonium Hydroxide {sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). Precaution--See 4.1. 26.1.2 Ammonium Oxalate, Saturated Solution (NH4)2 C204). ' 26.1.3 Potassium Permanganate, Standard Solution (0.1 N)--Dissolve 3.2 g of pure potassium permanganate (KMn04) in water and dilute to 1 L. Let stand 8 to 14 days, siphon off the dear solution (or filter through an asbestos filter), and standardize against NIST's standard sample 40c of sodium oxalate as follows: in a 400-mL beaker, dissolve 0.25 to 0.30 g (accurately weighed) of sodium oxalate in 250 mL of hot water (80 to 90C) and add 15 mL of sulfuric acid (H2S04, 1+1). Titrate at once with the KMn04 solution, stirring the liquid vigorously and continuously. The KMn04 must not be added more rapidly than 10 to 15 mL/min, and the last 0.5 to 1 mL must be added dropwise with particular care to allow each drop to be fully decolorized before the next is introduced. The temperature of the solution should not be below 60C by the time the end point is reached. (Too rapid cooling may be prevented by allowing the beaker to stand on a small asbestos-covered hot plate during the titration. The use of a small thermometer as a stirring rod is most convenient.) The weight of sodium oxalate used multiplied by 0.833 gives its iron equivalent. The KMn04 solution should be kept in a glass-stoppered bottle painted black to keep out light. 26.1.4 Sulfuric Acid {1+4)--Carefully mix 1 volume of concentrated sulfuric acid (H2S04, sp gr 1.84) (Precaution-- See 4.2) with 4 volumes of water. 26.2 Procedure: 26.2.1 Heat to boiling the united filtrate and washings, reduced in volume if need be, from the ZnS determination (see 25.2.2), add 1 mL of NH4OH and an excess of a hot saturated (NH4)2C204 solution. Continue the boiling until the precipitate becomes granular, let stand about 1 h, filter, and wash with hot water. Ignite, cool, and weigh as calcium oxide (CaO) (Notes 2, 12, and 13). Alternatively, place the beaker in which the precipitation was made under the funnel, pierce the apex of the filter with a stirring rod, and wash the precipitate into the beaker with hot water. Pour warm H2S04 (1+4) through the paper and wash a few times. Add about 30 mL of H2S04 (1+4), dilute to about 250 mL, heat to 90'C, and titrate at once with 0.1 N KMn04 solution (the temperature of the solution should not be below 60C when the end point is reached, see 25.1.3). Calculate to CaO (Notes 2, 12, and 13). (The iron equivalent of KMn04 X 0.502 = CaO value.) No t e 12--Care must be exercised in this washing, as 1 L of boiling water will dissolve over 0.01 g ofcalcium oxalate (CaC204). No t e !3--For more accurate work, the CaC204 precipitate should be ignited, cooled, cautiously moistened with water, redissolved in HQ, and the solution diluted to 100 mL. Add NH,OH in slight excess, boil the liquid, and filter and wash if a precipitate appeals. Reprecipitate the calcium with NH4OH and (NH4)2C204, as described in 25.2.1, filter, wash, ignite, cool, and weigh; or, titrate as described. 27. Soluble Magnesium 27.1 Reagents: 27.1.1 Ammonium Hydroxide {sp gr 0.90)--Concentrated ammonium hydroxide (NH4OH). Precaution--See 4.1. 27.1.2 Hydrochloric Acid {sp gr 1.19)--Concentrated hy drochloric acid (HCI). Precaution--See 4.2. 27.1.3 Hydrochloric Acid {1+3)--Mix 1 volume of con centrated HQ (sp gr 1.19) (Precaution--See 4.2) with 3 volumes of water. 27.1.4 Sodium Ammonium Phosphate, Saturated Solution (NaNH4HP04). 27.2 Procedure: 27.2.1 Acidify the filtrate from the calcium determination (see 26.2.1) with HCI, add 10 mL of a saturated solution of Na(NH4)HP04 and NH4OH dropwise, with constant stir ring. When the crystalline magnesium ammonium phos phate (Mg(NH4)P04 has formed, add 5 mL excess of NH4OH. Allow the solution to stand in a cool place for not less than 4 h, preferably overnight (Note 14). Filter and wash with water containing 2.5 % ammonia. Dissolve the precipi tate in a small quantity of hot HCI (1+3), dilute the solution to about 100 mL with water, add 1 mL of a saturated solution-of Na(NH4)HP04 and NH4OH dropwise, with constant stirring, until the precipitate is again formed, and then add 5 mL excess ofNH4OH. Let the precipitate stand in a cool place for not less than 2 h, filter on a Gooch crucible, wash with water containing 2.5 % of ammonia, ignite, cool, and weigh as magnesium pyrophosphate (MgP207) (Note 15). Calculate to magnesium oxide (MgO). No t e 14--The smaller the amount ofmagnesium present, the longer the precipitate must be allowed to settle. No t e 15--If the sample contained manganese, it will be caught in large part with the Mg2P207. Ifdesired, manganese may be determined by dissolving the Mg2P207. If desired, manganese may be determined by dissolving the Mg2P207 in nitric acid (Precaution--See 4.4) and applying the bismuthate method. 28. Carbon Dioxide 28.1 Determine carbon dioxide in accordance with Test Methods D 1301. 29. Total Soluble Sulfur Compounds (Note 2) 29.1 Determine total soluble sulfur in accordance with Methods D 34. This determination includes soluble sulfates, sulfur trioxide (S03) formed from sulfur dioxide, (S02), and the S03 that is formed from sulfide sulfur. 30. Soluble Sulfate (Note 2) 30.1 Determine soluble sulfates in accordance with Methods D 50-. 31. Sulfide Sulfur 31.1 Determine sulfide sulfur in accordance with Test Method D 2351. 33 DUP050297216 D 215 32. Sulfur Dioxide 32.1 Determine sulfur dioxide in accordance with Test Method D 2352. 33. Matter Soluble in Water 33.1 Determine matter soluble in water in accordance with Test Methods D 1208. No t e 16--The nature of the water-soluble matter may be deter mined by further examination, as the percentages of sulfur trioxide (S03) and calcium oxide (CaO) may be indicative. No t e 17--The water-soluble content of composite pigmentation, as determined in accordance with this method, is frequently higher than the sum ofthe water-soluble matter in the individual pigments. Possibly this is due to reaction in water between the individual pigments. 34. Calculation 34.1 The calculation of the component pigments of a mixed or combination pigment may be a somewhat difficult matter. Certain assumptions must be made, depending upon the complexity of the mixed pigment, as to the composition or formulas ofcomponent pigments and as to the manner in which the acidic and basic radicals are combined. Add any Al203(Fe203) found in the soluble portion to the siliceous matter and report the sum as "insoluble siliceous matter" unless the soluble aluminum is high; in this case, an aluminate is probably present, and the A1203 should be reported as A1203. Ifa small amount of soluble magnesium is found, it should also be added to the siliceous matter. If the soluble magnesium is high, the presence of MgC03 is indicated, and the MgO is calculated to MgC03 as described in 34.3. The insoluble siliceous matter reported should be based on the weight obtained on drying the total insoluble matter at 105*C ifthe combined water contained therein is to be considered. 34.2 Report Ti02 as Ti02, ZnS as ZnS, and BaS04 as BaS04. If CaC03, CaS04, BaC03, and MgC03 are absent, calculate C02 to basic carbonate white lead (Pb(C03)2 Pb(OH)2), and soluble S03 to PbS04. Calculate any excess of lead to PbO, add it to the PbS04, and report the sum as basic lead sulfate. Alternatively, multiply the sum of PbS04 + PbO by 0.058 to obtain the ZnO; add this result to the PbS04 + PbO and report as basic sulfate white lead. (The ZnO factor is based on the assumption that the average composition of commercial basic sulfate white lead is 78.5 % PbS04, 16.0 % PbO, and 5.5 % ZnO.) Lead oxide (PbO) should not be reported except in the presence of PbS04 unless the entire analysis is reported in the elementary or oxide form. 34.3 If the sample contains C02 but not soluble S03, calculate total lead to basic carbonate white lead (Pb(C03)2 Pb(OH)2); calculate residual C02 to CaC03, then to BaC03 and MgC03 if soluble barium and magnesium should be present in sufficient amounts to indicate the presence of these carbonates. The C02 result will be an index ofthis. A small amount ofresidual CaO is probably from the siliceous matter and should be added to the insoluble siliceous matter. 34.4 A small amount of soluble barium may be from the CaC03 used or may be due to the solubility of BaS04, if this compound is present in the original pigment This barium may be calculated to BaS04 and added to the BaS04 found in the insoluble matter. 34.5 If the sample contains soluble S03 but no C02, calculate CaO to CaS04 or CaS04 2H20; residual S03 to PbS04; add residual PbO to PbS04 and report the sum as basic lead sulfate. Alternatively, multiply PbS04 + PbO by 0.058 and add the result to the PbS04 + PbO, and report the total as basic sulfate white lead. 34.6 If the sample contains CaC03 (MgC03, BaC03) and also basic sulfate white lead, or CaS04 and basic carbonate white lead, or a mixture of these, it is not possible to determine or calculate the amount of PbC03 or PbS04 with any degree of certainty (see Notes 2 and 3). The presence of appreciable amounts of CaO and S03 in the water-soluble matter indicates the probable presence of CaS04 in the original pigment. The following arbitrary calculations may be made: calculate water-soluble S03 to CaS04 or CaS04*2H2O, subtract this S03 from total soluble S03, and calculate the remainder to PbS04; calculate residual CaO to CaC03> and then residual C02 to (PbC03)2-Pb(0H)2. If there is an excess of C02, calculate to MgC03 or BaC03, if the amounts of soluble magnesium and barium indicate the probable presence of these carbonates. Add residual PbO to PbS04 and calculate as described in 34.5 to basic sulfate white lead. 34.7 Report total antimony as Sb203. 34.8. Calculate sulfide sulfur to ZnS, subtract the zinc equivalent to the sulfur from the total zinc, then subtract the zinc required for the basic sulfate white lead, and report the remainder as ZnO. 34.9 Report directly the following: moisture and other volatile matter, loss on ignition, S02 and matter soluble in water. 35. Keywords 35.1 analysis ofpaint, white oil; analysis of pigment, white oil; lead analysis; white linseed oil paints, chemical analysis The American Society for Testing and Materials takes no position respecting the validity ol any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk Of infringement oi such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must bereviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invitedeither for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. 1. 5 1. quei liste N as a form by s nitre N< so in man perfc resul assui throi inter N< dure selec resul few estat 1. safe resf, prii bili 2. 1 2 B E E E E Paint Subc C: pub2li 34 DUP050297217 )le S03, te lead 03, then gnesium ate the m index from the nsoluble tom the >4) if this barium )4 found to C02, I SO3 to - sum as PbOby sport the '03) and irbonate ssible to >04 with ssence of r-soluble 4 in the ons may S04 or 503, and ICaOto OH)2. If iaC03, if icate the lPbOto c sulfate the zinc 'tract the port the d other luble in nt, white analysis Designation: D 333 - 87 (Reapproved 1991)e1 Standard Test Methods for Clear and Pigmented Lacquers1 This standard is issued under the fixed designation D 333; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovai. 61 No t e--Keywords were added editorially in April 1991. 1. Scope 1.1 These test methods cover procedures for testing lac quers and lacquer coatings. The test methods included are listed in Table 1. No t e 1--In accordance with Definitions D 16, a lacquer is defined as a coating composition that is based on synthetic thermoplastic film forming material dissolved in organic solvents) and that dries primarily by solvent evaporation. Typical lacquers include those based on nitrocellulose, other cellulose derivatives, vinyl resins, acrylic resins, etc. No t e 2--Lacquers may be applied under such diverse conditions, to so many different surfaces, and their dried films may be subjected to so many kinds ofwear and exposure that it is not possible to assure desired performance from a single selection of test methods and numerical results therefrom. Those skilled in lacquer technology may find partial assurance of obtaining desired qualities in various types of lacquers through careful selection of the methods covered herein and intelligent interpretation of results therefrom. No t e 3--It is intended ultimately to remove ail experimental proce dures from Test Methods D 333 and to establish them as a guide to the selection of test methods for lacquer and perhaps to interpretation of results therefrom. Temporarily there remain in Test Methods D 333 a few tests that are too short or otherwise presently unsuitable for establishment under separate ASTM designations. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: B 117 Method of Salt Spray (Fog) Testing2 D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products3 D56 Test Method for Rash Point by Tag Closed Tester4 D88 Test Method for Saybolt Viscosity5 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester4 1 These test methods are under the jurisdiction of ASTM Committee D-I on Print and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.55 on Factor-Applied Coatings on Preformed Products. Current edition approved June 26, 1987. Published August 1987. Originally Published as D 333 - 31 T. Last previous edition D 333 - 81. 2 Annual Book ofASTM Standards, Vols 03.02 and 06.01. ` Annual Book ofASTM Standards, Vols 06.01,06.02 and 06.03. 4 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 5 Annual Book ofASTM Standards, Vot 04.04. , D445 Test Method for Kinematic Viscosity of Trans parent and Opaque Liquids (and the Calculation of Dynamic Viscosity)6 D 522 Test Method for Mandrel Bend Test of Attached Organic Coatings7 D 523 Test Method for Specular Gloss7 D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products7 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces7 D658 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive7 D659 Method of Evaluating Degree of Chalking of Exterior Paints7 D 660 Test Method for Evaluating Degree of Checking of Exterior Paints7 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints7 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints7 D714 Test Method for Evaluating Degree of Blistering of Paints7 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints7 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels7 D 870 Practice for Testing Water Resistance of Coatings Using Water Immersion7 D968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive7 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers7 D1014 Test Method for Conducting Exterior Exposure Tests of Paints on Steel7 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base7 D1200 Test Method for Viscosity by Ford Viscosity Cup7 D1209 Test Method for Color of Gear Liquids (Plati num-Cobalt Scale)8 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems7 6 Annual Book ofASTM Standards, Vol 05.01. 7 Annual Book ofASTM Standards, Vol 06.01. 8 Annual Book ofASTM Standards, Vols 06.01 and 064)3. DUP050297218 n 1211 Test Method for Temperature-Change Resistance ofClear Nitrocellulose Lacquer Films Applied to Wood7 r>i308 Test Method for Effect of Household Chemicals on Gear and Pigmented Organic Finishes7 p 1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base7 p 1474 Test Methods for Indentation Hardness of Or ganic Coatings7 p 1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products7 D1535 Test Method for Specifying Color by the Munsell System9 pi544 Test Method for Color of Transparent Liquids {Gardner Color Scale)3 D1644 Test Methods for Nonvolatile Content of Var nishes7 p 1729 Practice for Visual Evaluation of Color Differ ences of Opaque Materials7 D1733 Method of Preparation of Aluminum Alloy Panels for Testing Paint, Varnish, Lacquer, and Related Products10 D1735 Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus7 D1737 Test Method for Elongation of Attached Organic Coatings with Cylindrical Mandrel Apparatus11 D2090 Test Method for Clarity and Cleanness of Paint and Ink Liquids12 D2091 Test Method for Print Resistance of Lacquers7 D 2199 Method for Measurement of Plasticizer Migration from Vinyl Fabrics to Lacquers7 D2204 Test Method for Perspiration Resistance of Or ganic Coatings13 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates7 D2620 Test Method for Light Stability of Clear Coatings7 D2805 Test Method for Hiding Power of Paints by Reflectometry7 D 3170 Test Method for Chipping Resistance ofCoatings7 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus14 E 308 Method for Computing the Colors of Objects by Using the CIE System9 3. Significance and Use 3.1 These test methods are intended to compile as well as provide screening tests in evaluating clear and pigmented lacquers as used in different coating operations. 3.2 Each coating system may contain from a simple one coat operation to a multicoat finishing system. 3.3 The substrates may be varied, ferrous and non ferrous, plastic or wood which can affect the performance of a given coating system. 3.4 Substrate cleaning, chemically or physically, is an TABLE 1 List of Test Methods Test Method Section General Requirements Liquid Materials: Color of Clear Lacquers: Gardner Color Scale Platinum-Cobalt Scale Rash Point Tag Closed Cup 5 10 10 12 Homogeneity: Clarity and Cleanness Fineness of Pigment Grind Nonvolatile Matter Sample Preparation Viscosity: Ford Cup (Efflux) Kinematic High Precision Weight per Gallon (Density) Dried Films: Abrasion Resistance: Air Blast Abrasion Tester Falling Sand Method Chip Resistance: Color-Pigmented Coatings: Spectrophotometric Method Munsell Color System Color Difference-Pigmented Coatings: Visual Method Instrumental Evaluation of Color Differences of Opaque Materials Elongation: Conical Mandrel Cyindrical Mandrel Film Thickness: Nondestructive Magnetic Base Nondestructive Nonmagnetic Metallic Base Penetration Thickness Gage Dial Comparator Gloss; Specular Gloss Hardness Indentation Method Hiding Power Household Chemical Resistance light Stability Outdoor Exposure: Preparation of Coated Panels: Aluminum Alloy Panels Steel Panels Test Procedures: Exposure Tests Using Steel Panels Evaluating Blistering Evaluating Chalking Evaluating Checking Evaluating Cracking Evaluating Rusting Evaluating Erosion Evaluating Flaking Panel Preparation: Manual Spraying Method Automatic Application Plasticizer Migration Print Test Salt Fog Temperature-Change Resistance Water Fog Testing Water Immersion Test 9 9 8 6 It 11 7 20 20 30 16 16 17 17 18 18 14 14 14 14 15 19 28 22 31 , 23 23 23 23 23 23 23 23 23 23 13 13 30 21 25 24 26 27 ASTM Method D 1544 D1209 D 56, D 93, D 3278 D2090 D1210 D1644 D 1200 D445 D1475 D658 D968 D3170 D 308 D 1535 D 1729 D 2244 D 522 D 1737 D 1186 D 1400 D 1400 D1005 D523 D 1474 D 2805 D1308 D2620 D1733 D609 D 1014 D714 D 659 D 660 D 661 D 810 D662 D 772 0 823 D2199 D 2091 B 117 D 1211 O 1735 D870 * Annual Book ofASTM Standards, Vol 14.02. Discontinued: see 1979 Annual Book ofASTMStandards, Part 27. 11 Discontinued; see 1988 Annual Book ofASTM Standards, Vol 06.01. ia Annual Book ofASTM Standards, Vols 06.02 and 06.03. Discontinued: see 1976 Annual Book ofASTM Standards, Part 27. 14 Annual Book ofASTM Standards, Vol 06.03. essential and critical aspect to the performance ofthe coating system. 3.5 Results from the various tests are not necessarily all useful in evaluating the performance ofthe different types of coating systems used on the many varied substrates. 4. 4 sun rek 5. c tair bot pac me tret test 6. 6 Dl vise spe cup gall 7. : 7 the in i filir hen frot tem 7 dest mei wel Me dan 8. 1 8 uni ma 8 in i lacc 8 ferr. titai Tes 9. ( 9. indi cole cert- 9. Test cole 9. quei shal havt DUP050297219 ,STM ethod 1544 1209 56, 33, 3278 2090 1210 H644 >1200 >445 >1475 >658 1968 13170 1308 11535 11729 12244 1522 31737 11186 11400 31400 11005 3523 11474 3 2805 11308 32620 31733 1609 1014 714 659 660 661 610 >662 3 772 623 D2199 2091 8117 1211 D1735 0 870 e coating sarily all t types of 0 333 4. General Requirements 4.1 All tests shall be made in diffused light (not in direct sunlight), and at 73.5 3.5T (23 2C) and 50 5 % relative humidity, unless otherwise specified. 5. Preparation of Sample 5.1 Many clear lacquers and all pigmented lacquers con tain suspended solids that have a tendency to settle to the bottom of the container. Stir any settled portion with a paddle or spatula and then shake vigorously for 10 min on a mechanical agitator. Since many lacquer solvents are ex tremely volatile, care should be taken during sampling and testing to avoid loss of significant amounts of volatile matter. 6. Weight Per Gallon 6.1 Determine the density as described in Test Method D 1475. This method is particularly adaptable for highviscosity fluids or where a component is too volatile for a specific gravity balance determination. If a weight per gallon cup of 83.2-mL capacity is used, calculation of weight per gallon is simplified. 7. Nonvolatile Matter 7.1 Nonvolatile matter determination is an indication of the amount of permanent film-forming material contained in a lacquer. At ambient temperatures, drying of a lacquer film may involve gradual loss of slowly volatile solvents, hence solids determinations may differ from those resulting from a nonvolatile determination accelerated by a higher temperature. 7.2 Determine the nonvolatile content of lacquers as described in Test Methods D 1644. As an additional require ment, the specimen shall be reheated and reweighed until the weight is constant to within 1 mg. Test Method A of Test Methods D 1644 is preferred since Method B is potentially dangerous when used with lacquers. 8. Homogeneity 8.1 Good quality lacquers and their ingredients should be uniformly constituted and free from particles of foreign matter. 8.2 Determine the presence or absence of foreign matter in nonpigmented liquids for use in paints and lacquers or lacquers themselves as described in Test Method D 2090. 8.3 Determine the degree of dispersion (commonly re ferred to as "fineness of grind") of pigment, semiquanlitatively, in pigmented coating systems in accordance with Test Method D 1210. 9. Color 9.1 The color of a clear lacquer is only a preliminary indication of the color of a dried film of lacquer. The initial color may bleach and another color may appear under certain conditions of exposure. 9.2 Determine the color of clear lacquers as described in Test Method D 1544. This method gives a comparison ofthe color of the sample with that of a color reference standard. 9.3 Determine the color of essentially water-white lac quers in accordance with Test Method D 1209. This method shall be used where the color-producing bodies in the lacquer have very nearly the same light-absorption characteristics as those of the platinum-cobalt standards. 10. Viscosity 10.1 The viscosity of a lacquer is a property that can be used as a guide in determining the ease with which a given lacquer may be applied. For example, lacquers designed for spray application may be low in viscosity whereas they are high for doctor blade or roller application. 10.2 Determine the viscosity of clear and pigmented finishes designed for spray application as described in Test Method D 1200. This method is not recommended for lacquers with viscosities requiring more than 100 s efflux time. 10.3 For precise viscosity determinations in the range from 0.4 to 16 000 cSt proceed in accordance with Test Method D 445. N' 4--Caution should be observed in that it is recognized that changes in viscosity may occur in lacquers upon aging. 11. Flash Point 11.1 The organic solvents used in lacquers have character istic flash points. The flash point of a liquid is defined as the lowest temperature, corrected to 101.3 kPa (760 mmHg) of pressure, of the sample at which application of an ignition source causes the vapor of the sample to ignite under specified conditions of test. 11.2 Determine the flash point by Test Method D56 or Test Methods D 93 for liquid storage regulations of Occupa tional Safety and Health Administration (OSHA) of U. S. Department of Labor and for classification of hazardous liquids for shipments under the regulations of U. S. Depart ment of Transportation and bulk shipments by water. 11.2.1 Determine the flash point of lacquer or lacquer materials having a viscosity less than 9.5 cSt at 77F (25C) or 45 SUS at 100T (37.8C) (Method D 88) by Test Method D 56 and of lacquers having a viscosity of more than 9.5 cSt at 77F (25C) or 45 SUS at 100F (37.8Q by Method A of Test Methods D 93. Use Method B of Test Methods D 93 whenever there is a question that the heat transfer within a viscous lacquer is not sufficient to assure an accurate flash point. In addition, use Method B when testing pigmented lacquers or suspensions of solids and liquids which tend to skin under test conditions. 11.3 Test Methods D 3278, which give comparable results to Test Method D 56 and Test Methods D 93 while requiring a smaller specimen and less time to run, may be used as an alternative method. 12. Panel Preparation 12.1 In the evaluation ofcoated panels a uniform dry film thickness of lacquer is essential in order to eliminate any effect due to film thickness. Unless otherwise specified, the dry film thicknesses shall be as follows: Mils Micrometres Lacquer primer Lacquer primer surfacer Clear lacquer Gloss pigmented lacquer Lacquer putties 0.3 to 0.6 1.0 to 2.0 l.Oto 1.2 1.0 to 1.2 4.0 to 6.0 8 to 15 25 to 50 25 to 31 25 to 31 100 to 150 12.2 Panels may be prepared by either manual or auto matic application of lacquers. First reduce lacquers with the DU P050297220 D 333 specified thinner (if reduction is required) to the required dilution solids or viscosity. If no viscosity is specified, spray with standard-type guns at a viscosity of 17 to 25 s in a No. 4 Ford Cup at 25C determined as described in Test Method D 1200. 12.3 Cold Spray--In manual application by cold spray, keep the air pressure constant and provide the air line with a moisture trap. Adjust the flow, gun distance from test panel, and spray pattern that the deposited film is kept smooth, level, and wet. Apply the number of coats or thickness, or both, specified in the product specification. 12.4 Hot Spray--The packaged material shall be applied with hot spray equipment approved by the Underwriter's Laboratory. When dilution is necessary, the material shall be reduced with the specified thinner to the viscosity required for hot spray application. The conditions of operation with respect to temperature of the heating unit, type of spray gun, atomization pressure and pressure on feed tank type,, adjust ment of air cap and fluid tip, distance of gun from work, and rate of flow of material at the spray nozzle shail be 9s agreed upon between purchaser and seller. 12.5 Automatic Application--Four methods of applying films of uniform thickness automatically are described in Test Methods D 823. The methods are as follows: Test Method A--Automatic Spraying Machine, Test Method B--Automatic Dip-Coater, Test Method C--Automatic Blade Film Applicator, and Test Method D--Motor-Driven Blade Film Applicator. 13. Film Thickness 13.1 Many properties of lacquer films vary with the thickness of the dry film. The measurement of dry film thickness may be accomplished with various apparatus depending upon the substrate to which the film is applied. Three nondestructive methods of thickness determination are given for films that are not easily removable from their substrate and thus do not lend themselves to simple mea surement with a constant-pressure micrometer. Two destruc tive methods are given. The methods are as follows: 13.2 Nondestructive Methods: 13.2.1 Test Method D 1186. This method is also recom mended for thin films, less than 0.5 mil (0.005 in.) (0.013 mm) in thickness. 13.2.2 Test Method D 1400, Method A. By the use of plastic shims of known thickness, the film thickness can be estimated to approximately 10 % 13.2.3 Test Methods D 1400, Method C. 13.3 Destructive Methods: 13.3.1 Test Methods D 1005. 13.3.2 Test Methods D 1400, Method B. 14. Gloss 14.1 This property relates to that aspect of the reflecting properties of a coating as determined by the brightness and configuration of reflected images. 14.2 Determine gloss of nonmetallic finishes in accord ance with Test Method D523. This method covers the measurement of the amount of light reflected specularly from a film's surface. While this property is a function of film gloss, correlation with visual observations is not always obtained. 15. Color-Pigmented Coatings 15.1 The colors of opaque objects such as painted surfaces may be specified using visual or instrumental means. 15.2 By visual means the colors of painted surfaces in terms of the Munsell Color System may be determined i accordance with Test Method D 1535. This method provides a simple alternative to the more precise and more compli cated method of color specification based on spectropho tometry. 15.3 By spectrophotometer, either visual or photoelectric types, the colors of light-reflecting coatings and spectral characteristics may be determined using Method E 308. 16. Color Difference-Pigmented Coatings 16.1 The small daylight color differences between two similarly homogeneously colored, opaque objects such as painted surfaces may be determined using visual evaluating techniques or by instrumental means. 16.2 Determine by visual evaluation color differences of opaque materials using Practice D 1729. This practice spec ifies characteristics of light sources, illuminating and viewing conditions, size of specimens, and general procedures. 16.3 Determine small daylight color differences between opaque paint specimens in accordance with Method D 2244. This test method correlates reasonably well with visuai judgments of character and perceptibility of color differences provided specimens are illuminated and viewed under con ditions substantially the same as used in the instrument For nonfluorescent opaque paint specimens or materials that do not contain metallic pigments ("bronze" powders and alu minum powders) or "pearly" pigments or other materials that produce optical phenomena that contribute to the visual effect, test in accordance with Test Method D 2244. 17. Elongation 17.1 An elongation test may be used as an indication of the flexibility of an attached organic coating. It can also show whether there is any change during aging. 17.2 Determine the elongation of attached organic coat ings when applied to flat sheet metal of uniform surface texture in accordance with Test Method D 522 or Test Method D 1737. 18. Hardness 18.1 Determine film hardness of lacquers applied to plane rigid surfaces in accordance with Test Method D 1474. In this method the resistance of a coating to penetration by an indenter is measured and converted to a hardness value. 19. Abrasion Resistance 19.1 Determine the abrasion resistance as described in either Test Method D658 or Test Method D968. Both methods cover measurement of the resistance to abrasion of coatings applied to metal panels. 20. Print Test 20.1 A print test can be used to determine two character istics of a film. If a film is thoroughly dry, the test will give a measure to the susceptibility of the film itself to press*-' marring. However, as the test is used in a product!11' situation, it can be used to determine the degree to which 8 38 film has be safel 20.2 Test Me 1. Hoi 21.1 anic cc 22. Out 22.1 i exposun applicati refinish, tested a Experier a marke several / strate vt uniform evaluatii 22.2 J anticipat should 1 following 22.2.1 22.2.2 22.2.3 22.3 i ings shot exposure follows: 22.3.1 22.3.2 22.3.3 22.3.4 22.3.5 22.3.6 22.3.7 23. Tern or DUP050297221 film has released solvents and hence whether'the product can be safely packed. 20.2 Determine imprinting of dried films as described in Test Method D 2091. 21. Household Chemical Resistance 21.1 Household chemicals may alter the surface of or ganic coatings, for example through discoloration, change in gloss, blistering, swelling, and loss of adhesion. 21.2 Determine, qualitatively, the effects of household chemicals in accordance with Test Method D 1308. 22. Outdoor Exposure 22.1 It is important to determine the resistance to outdoor exposure of lacquers destined for exterior use prior to their application to surfaces which may be difficult or costly to refinish, or both. Systems of primer and lacquer should be tested as a whole rather than as separate components. Experience indicates that the type of substrate employed has a marked bearing on weathering results. It is the purpose of several ASTM methods to minimize the influence of sub strate variation by providing uniform panel selection and uniform procedures for conducting exposure tests and for evaluating and recording results. 22.2 Preparation of Panels--Depending on the substrate anticipated to be coated, panels for outdoor exposure testing should be prepared and tested in accordance with the following methods: 22.2.1 Test Method D 1733. 22.2.2 Methods D 609. 22.2.3 Method D 1014. 22.3 Test Procedures--Many properties of organic coat ings should be evaluated periodically throughout the outdoor exposure period. These properties may be evaluated as follows: 22.3.1 Blistering--Test Method D 714. 22.3.2 Chalking--Method D 659. 22.3.3 Checking--Test Method D 660. 22.3.4 Cracking--Test Method D 661. 22.3.5 Rusting--Method D 610. 22.3.6 Erosion--Test Method D 662. 22.3.7 Flaking--Test Method D 772. 23. Temperature-Change Resistance 23.1 A test for resistance to temperature change, or a cold cracking test (as it is sometimes called), is designed to give an indication of the resistance of a coating system to fracturing or checking, caused both by changes in temperature and humidity and by age. The degree of correlation between test results and long-term room temperature aging varies with the type of lacquer. The industry uses the test widely and feels that systems showing good cold crack resistance usually will give satisfactory performance in service. Some factors that can affect results are the type of substrate, its thickness, the rate at which the individual panels are cooled, the film thickness, and the nature of any priming or sealer coats. 23.2 Determine the temperature-change resistance in ac cordance with Test Method D 1211, This method specifies that the test panels be aged ID days. If the panels are much ider than this, the resistance to checking is expected to be less and sometimes considerably so depending on the nature of the film. 24. Salt Fog 24.1 Salt spray (fog) testing of lacquers applied to metal substrates is helpful in determining their resistance to failure in service under atmospheric conditions that might prevail in sea coast areas. 24.2 Under accelerated conditions of laboratory testing, only the temperature, the pH, or concentration of the salt solution, and other physical properties can be controlled, the selection of the substrate, the coating technique, the manner in which the coating is scribed (parallel or X's), the location or position of the panels within the cabinet, the length of the test, the inspection of the panels, and the method of reporting results must generally be as agreed upon between purchaser and seller. Systems of primer and lacquer should be tested as a whole rather than as separate components. 24.3 Determine the salt spray resistance as described in Method B 117. 25. Water Fog Testing 25.1 Water fog testing of lacquers is helpful in deter mining their resistance to failure in service under conditions of high humidity. Failure is usually evidenced by blushing, dulling, blistering, or excessive softening that does not disappear upon evaporation of the absorbed water. Systems of primer and top-coat lacquer should be tested as a whole rather than as separate components. The use of unrealisti cally short drying times or excessively low temperature bakes will give erratic and misleading results. 25.2 Determine resistance to failure under conditions of high humidity in accordance with Test Method D 1735. 26. Water Immersion Testing 26.1 Water immersion testing is best suited for testing lacquers or systems that will actually be soaked in water during service. Materials that will be subjected to humid atmospheres only should be subjected to water fog testing. Failure is usually evidenced by blushing, dulling, blistering, or excessive softening that does not disappear upon evapora tion of the absorbed water. 26.2 Determine, in an accelerated manner, the resistance to failure of a coating immersed in water in accordance with Practice D 870. 27. Hiding Power 27.1 Hiding power of chromatic and non-chromatic coat ings can be determined using Test Method D2805. 28. Perspiration Resistance 28.1 The effects of human perspiration on the surface of organic coatings are varied. The coating may undergo an objectionable alteration in surface appearance such as discol oration, loss of gloss, blistering, wrinkling, or roughening. The coating may lose adhesion, soften, become embrittled, or any combination of these changes may take place. 28.2 Determine the effects of perspiration on organic coatings in accordance with Test Method D2204. This method covers an accelerated procedure for determining the resistance to failure of organic coatings on metallic panels 39 DUP050297222 D333 #hen exposed to human perspiration. 29, Plasticizer Migration 29.1 Plasticizers used in vinyl fabrics may migrate into lacquer Sims that come in contact with the fabric and cause objectionable marring and softening of the lacquer film. 29.2 Determine the tendency for plasticizer to migrate in accordance with Test Method D 2199. 30. Chip Resistance 30.1 Chip resistance testing is useful for determining the ability ofthe coating or coating system, or both, to withstand flying stones or other objects. Systems of primer and topcoat should be tested as a system rather than as separate compo nents. 31. Light Stability of Clear Coatings 31.1 The ability of clear coatings not to change color upon exposure to sunlight is an important characteristic, especially over white or light-colored substrates. Coatings for indoor use may be tested in accordance with Test Method D 2620. 32. Keywords 32.1 clear lacquers; pigmented lacquers The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is sub/ect to revision at any time by tbe responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressedto ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you teet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. i 1. Scope un quantita test pain 1.2 T tion pm other m 1.3 I cttions, address the resj appropr applicai 2. Reft 2.1 , D 16 an D 14 qu D17 of D28 R E 9' 4! F 3. Te 3.1 3.1. refer t 3.2 3.2 tion c powe 3.2 rate c 1T) and K mittee DUP050297223 coat ipo- ipon ially door 520. Designation: D 344 - 89 Standard Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts1 This standard is issued under the fixed designation D 344; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method provides for the qualitative and quantitative visual determination of the hiding power of a test paint relative to that of a comparison paint. 1.2 This test method describes only a brushout applica tion procedure in specific detail, but its concepts are valid for other methods of application as well. ' 1.3 This standard may involve hazardous materials, operi ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products3 D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials4 D2805 Test Method for Hiding Power of Paints by Reflectometry3 E97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry5 3. Terminology 3.1 Definitions: 3.1.1 For definitions of terms used in this test method, refer to Definitions D 16 and the Paint/Coatings Dictionary.6 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 relative hiding power, qualitative--the characteriza tion of a test paint as being better, equal, or poorer in hiding power than a comparison paint. 3.2.2 relative hiding power, quantitative--the spreading rate of a paint expressed as a percent of the spreading rate of 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DOl.26 on Optica] Properties. Current edition approved May 26, 1989. Published August 1989. Originally published as D 344 - 32. Last previous edition D 344 - 84. Annua/ Book ofASTM Standards, Vols 06.01, 06.02. and 06.03. ' Annua/ Book ofASTM Standards. Vol 06.01. 'Annual Book ofASTMStandards, Vol 14.02. 5Annual Book ofASTM Standards, Vols 06.01 and 14.02. * Published by the Federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. a comparison paint at equal hiding. 4. Summary of Test Method 4.1 Qualitative--The test and comparison paints are brushed out uniformly at the same spreading rate on black and white hiding power charts. After drying the brushouts are compared visually to see which paint has been most effective in reducing the substrate contrast. 4.2 Quantitative--Additional brushouts are made with the comparison paint, if and as necessary, to determine the spreading rate at which it matches the hiding ofthe test paint brushout. 5. Significance and Use 5.1 This test method evaluates the hiding power of a test paint relative to a comparison paint. The results have significance only within that relationship. It may be used for production control or quality comparisons. 5.2 When a paint is applied by brush or any other practical method, the opacity of the film is affected by variations in film thickness related to the application proce dure and to the application characteristics of the paint. Two paints that hide equally well by this method might therefore differ considerably when applied with a doctor blade, since the latter method gives essentially perfect leveling. Different brushes or surface application conditions can likewise give different results. No t e 1--Test Method D 2805 describes an instrumental method for quantitatively determining hiding power without reference to a material paint standard. The paint film is applied at a uniform thickness (for example, with a doctor blade), the film thickness is measured rigorously, and the opacity is evaluated photometrically. Hiding power is thereby determined with a high degree of precision. 5.3 Test Method D 344 is less precise than Test Method D 2805, but is more practical because it is responsive to the application characteristics ofpaints and is simpler in concept and execution. 6. Apparatus 6.1 Balance, top-loading laboratory balance having a capacity of 100 g and sensitivity of 0.1 g. 6.2 Syringe, 10-mL capacity. 6.3 Paint Brush, ferrule 2 in. (50 mm) wide and 9/m in. (14 mm) thick, tapered polyester filaments 2% in. (70 mm) long with flagged chisel trim tip.7 7 Describes the Leneta-EZ Painter Certified Standard Paint Brush used by the round-robin participants,, available from Leneta Company, P. O. Box 86, Ho-Ho-Kus, NJ 07423. Equivalent brushes may be used. DUP050297224 D 344 6.4 Container, */2-pint can or 250-mL beaker. 6.5 Test Surface, a smooth-surfaced paper chart having adjacent black and white areas and coated with a suitable varnish or lacquer so as to render the surface impervious to paint liquids. The black and white areas of the chart shall have luminous reflectance factors of 1 % maximum and 75 % minimum, respectively, when tested in accordance with Test Method E 97. The white areas of the charts used in any one testing program shall not differ in their reflectance factors by more than 1 %. Any suitable regular design of contrasting areas may be used. The chart8 shall have a defined test area of 0.1 m2. Larger test areas may be used if available, with appropriate modification of the indicated calculations. 6.6 Illumination, a light source providing diffuse light of reasonable intensity, preferably northern sky light or an approximation of same. (See Practice D 1729). 7. Preparation of Brushouts 7.1 Select a convenient and suitable spreading rate, mutu ally agreeable to all parties involved in the testing program, and preferably in the range from 400 to 800 ft2/gal (9.8 to 19.6 m2/L). In any case, the spreading rate shall not be so low that the substrate contrast is difficult to see nor so high that it is difficult to apply the paint at a reasonably uniform film thickness. No t e 2--The gallon unit referred to here and throughout this test method is the U.S. gallon (3785.4 mL). 7.2 Determine the density D in grams per millilitre of the comparisons and test paints, in accordance with Test Method D 1475. 7.3 Calculate to three significant figures the volume V in millilitres to apply for the selected spreading rate SR as follows: Vi n_ 100 4074.6 ( ' SR{m2/L) R(ft2/gal) 7.4 Calculate to three significant figures, the weight W in grams corresponding to the volume K(mL) as follows: W(g) = P(mL) x >(g/mL) 7.5 To prepare a brushout, first stir the paint well. Then precondition the brush by dipping it into the paint and working it out on a smooth, nonporous surface. Take up the desired volume of paint in the syringe and weigh it with the brush in the empty container. Place the test chart on a level bench top, distribute the paint from the syringe all around onto the test area of the chart, then brush the paint out uniformly within the test area. Set the brushout aside to dry in a horizontal position, protected adequately from dust and under normal room conditions of ventilation and tempera ture. Reweigh the empty syringe with the brush and con tainer. The loss of weight represents the actual weight of paint applied to the test surface as opposed to the intended weight calculated from 7.3 and 7.4. If there is a discrepancy do not attempt to correct it by removing or applying paint6 6 Suitable charts are available from Lenela Company, P. O. Bos 86, HoHo-Kus, NJ 07423. since this would disturb the leveling of the brushout. Instead, calculate the actual spreading rate as follows: SRa ~ ^ * SRB where: SRa = actual spreading rate, B -- intended weight, A -- actual weight, and SRb -- intended spreading rate. 8. Evaluation Procedure 8.1 Viewing conditions--When the test and comparison paint brushouts are thoroughly dry, place them vertically side by side against a flat surface and view them from a distance of 5 to 10 ft (1.5 to 3 m) under illumination conditions as described in 6.6. 8.2 Qualitative Evaluation: 8.2.1 If the contrast between the black and white areas of the test paint brushout is adjudged less than, equal to, or more than that of the comparison paint brushout, then the hiding power of the test paint is considered as better than, equal to, or poorer than that of the comparison paint. 8.2.2 If the actual spreading rate of the lower contrast paint-out is lower than that of the other paint-out by more than 3 %, prepare a second brushout with either paint so as to eliminate the difference, then compare again to confirm or revise the previous estimation of relative hiding power. 8.3 Quantitative Evaluation: 8.3.1 If the hiding of the test paint brushout does not match that of the comparison paint at the same spreading rate, make a series of additional comparison paint brushouts at several other spreading rates, differing in steps of approx imately 15 % and providing contrasts above and below that of the test paint brushout. Refer to these and to the original comparison paint brushout as standards. If the standards are prepared correctly each increase in spreading rate will correspond to a perceptible increase in contrast. Compare the standards under the viewing conditions described in 8.1 to assure that this is the case. 8.3.2 Compare the brushout of the test paint with the standards under the specified viewing conditions to deter mine which standard it matches in contrast or, if none, to which pair of successive standards it is intermediate. In the latter case view the test paint brushout with the two standards on either side and rate the contrast ofthe test paint brushout by estimating the contrast difference between it and the lower spreading rate (lower contrast) standard, as a fraction of the contrast difference between the two standards to the nearest fourth. Keeping the test paint brushout in the middle, reverse the position of the two standards and rate the test paint brushout again in the same way. The final rating is the mean of the two to the nearest eighth. 8.3.3 Calculate the spreading rate (SRC) of the compar ison paint at which it is estimated to match the hiding of the test paint brushout as follows: SRc=SR, + X(SR2 - SRJ where: SR i = spreading rate of the lower spreading rate (lower contrast) standard. 42 SR2 -- X -8.3.4 in acci where: HP, = SRt = SR, = 9. Rep' 9.1 ( power < than th such tei as may 9.2 ( power c is a purt per gall 10. Pre 10.1 compare laboratc trials. T a paint the com iseffecti appropr these tes 10.2 < DU P0502 97225 nstead, - parison :rtically from a ination areas of 1 to, or hen the jr than, t. contrast >y more nt so as ifirmor er. oes not treading ushouts approxow that original ards are ate will ompare d in 8.1 ith the deterone, to In the ie two .st paint ;n it and :d, as a tandards at in the i rate the rating is comparng of the 0 344 SR2 - spreading rate of the higher spreading rate (higher contrast) standard, and X - fractional contrast rating of the test paint brushout. 8.3.4 Calculate the relative hiding power of the test paint in accordance with the definition in 3.2.2 as follows: where: HPt - relative hiding power of the test paint, SRt = spreading rate of the test paint, and SRC spreading rate of the comparison paint at equal hiding, as determined by an actual match with one of the standards or by estimation between two standards as described in 8.3.2. 9. Report 9.1 Qualitative (see 8.2)--Report the relative hiding power of the test paint as better than, equal to, or poorer than the comparison paint. The report may be amplified by such terms as exactly, slightly, moderately, considerably, etc., as may seem appropriate. 9.2 Quantitative (see 8.3)--Report the relative hiding power of the test coating to the nearest whole number. This is a purely numerical value. Physical units such as square feet per gallon or square metres per litre are not applicable. 10. Precision 10.1 Qualitative--Four test paints were rated versus a comparison paint by three laboratories, twice each by one laboratory and once each by the other two, for a total of 16 trials. There was only one discrepancy, which occurred with a paint that was apparently very similar in hiding power to the comparison paint. These results indicate that the method is effective, but more results would be required to develop an appropriate precision statement. Table 1 gives the results of these tests. 10.2 Quantitative--In an interlaboratory study of this TABLE 1 Round Robin Results of Relative Hiding Power of Four White Paints versus a Comparison White Paint Method Qualitative Quantitative Paint VI V2a V3 V4 V5 VI V28 V3 V4 V5 Laboratory 1 Trial 1 A Trial 2 A CC CC AC 125 117 100 100 85 93 66 82 102 90 Laboratory Laboratory 23 AA CC CC cc 115 120 100 100 62 96 60 67 83 95 * Indicates that the test paint hides better than the comparison paint. 8 Comparison paint, relative hiding power equals 100. 0 Indicates that the test paint hides poorer than the comparison paint method four coatings were evaluated for hiding power against a fifth coating taken as the standard. In one labora tory each material was tested twice, but only once in the other two laboratories. Statistical analysis of the results revealed that the two results for each coating from the one laboratory were as variable as those from the other two. Consequently, the two results were treated as being indi vidual results and the between-laboratory standard deviation was found to be 10 % with 12 df. Based on this standard deviation, the following criterion should be used forjudging the acceptability of results at the 95 % confidence level: 10.2.1 Reproducibility--Two single results obtained by operators in different laboratories should be considered suspect if they differ in relative hiding power by more than 32 %. 10.2.2 Repeatability--A reasonable estimate of withinlaboratory precision could not be obtained because only one laboratory repeated the test. However, the repeatability should be similar to the reproducibility. 11. Keywords 11.1 hiding power; relative hiding; opacity The American Society for Testing and Materials takes no position respecting the validity oI any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either hr revision of this standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration af a meeting of the responsible technical committee, which you may attend. If you tee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. & (lower DUP050297226 Designation: D 358 - 83 {Reapproved 1988) Standard Specification for Wood to Be Used as Panels in Weathering Tests of Coatings1 This standard is issued under the fixed designation D 358; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapprovai. This standard has been approvedfor use by agencies ofthe Department 0/Defense to replace Method 2031 ofFederal Test Standard No. 141. Consult the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department ofDefense. 1. Scope 1.1 This specification designates woods for weathering tests of exterior solvent-borne or water-borne paints and other materials of similar purpose. Such tests may include either outdoor exposure tests or accelerated laboratory tests. It is the purpose of this specification to minimize the influence of variation of wood of a given species on test results. 2. General Considerations 2.1 A variety ofdifferent species should be used for testing finishes because of the wide variations in the anatomy and the density between wood species. The factors have tremen dous influences on finish performance. Latewood band width and density are especially important to finish perform ance, and these parameters vary significantly between wood species. Cedar and redwood have relatively low proportions of hard summerwood distributed in narrow bands and contain extractives that discolor some paint films. Southern pine has a large proportion of hard summerwood in wide bands. 2.2 The angle between the growth rings and the surface of the specimen is very critical to finish performance. Commer cial practice utilizes the following classification system. Boards in which growth form an angle of less than 30" with the wide surface of the piece are said to be flat-sawn or flat-grained; those with the rings intersecting at angles between 30and 60are termed bastard-sawn; and those with angles greater than 60 are termed quarter-sawn, edge grain, or vertical grain. WESTERN RED CEDAR 3. Species 3.1 The material for test panels shall be western red cedar (Thuja plicata). 4. Weight per Volume 4.1 When the wood is in equilibrium with air at 60 to 65 % relative humidity and 70 1F (21 0.5C) it shall weigh 22 to 23 lb/ft3 (350 to 370 kg/m3) or at 50 5 % relative humidity and 73.5 3.5"F <23 2C), which are 1 This specification is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility DO 1.52 on Factory-Coated Wood Products. Current edition approved Oct. 28, 1983. Published December 1983. Originally published as D 358 - 33. Last previous edition D 358 - 77. specified in Specification D 3924 as standard conditions for testing paint and related coatings, it shall weigh 21.4 to 22.4 lb/ft3 (343 to 359 kg/m3). No t e 1--The density requirement is to eliminate wood specimens that vary greatly from the average for that species. Either set of conditions may be used to establish the density. At 60 to 65 % relative humidity wood has a moisture content of approximately 12 % while at 45 to 55 % relative humidity it contains 9 to 10 %. The former is closer to the moisture content of wood exposed to most exterior climatic conditions. 5. Character of Wood 5.1 The wood shall be heartwood having edge grain and shall be free of knots and other defects. The color of the wood shall be uniform across each panel with no streaks that are excessively light or dark. The number of annual growth rings per inch along the radius of the log from which the wood was obtained shall not be less than ten. The surfaces shall be smoothly planed and sanded thoroughly with 150 grit sandpaper within two weeks of testing. 6. Thickness of Panels 6.1 The minimum thicknesses (Note 2) in proportion to width (across the grain) shall be as follows: Panel Width, in. (mm) Minimum Thickness, in. (mm) Less than 3 (less than 75)' 3 to 6 (75 to 150) Over 6 (over 150) Vs (10) Vt(U) y< (19) No t e 2--Minimum thicknesses in proportion to width (across die grain) do not apply to panels made ofclapboard or siding ofcommercial types, which shall be used as regularly marketed. WHITE PINE AND PONDEROSA PINE 7. Species 7.1 White pine wood shall be northern white pine (Pinus strobus). Western white pine (Pinus monticola), or sugar pine (Pinus lambertiana). Western white pine is sometimes called Idaho white pine. Ponderosa pine wood shall be Pinus ponderosa. 8. Weight per Volume 8.1 When the wood is in equilibrium with air at 60 to 65 % relative humidity and 70 1F (21 0.5C) it shall weigh 23 to 27 lb/ft3 (370 to 430 kg/m3) or at 50 5 % relative humidity and 73.5 3.5F (23 2C) it shall weigh 22.4 to 26.4 lb/ft3 (359 to 423 kg/m3). (See Note 1.) 9. Ch 9.1 other each i The m of the than 1 thorou testing 9.2 as desi bark si 10. Tl 10.1 to widi i 3 C 11. Sp. 11.1 (Pinus limited ments p 12. We 12.1 65% re weigh 3 relative 31 to 37 13. Cba 13.1 ' other de each pai The nur of the lo than 4 < planed within tv 13.2 1 ; 14. Thlc 14.1 1 ; to width Pi Les.* : : 3 to Ove IS. Speci 15.1 T (Sequoia DUP050297227 ms for o 22.4 sciraens set of relative while at is closer climatic tin and of the iksthat growth ich the surfaces ith 150 rtion to , in. t o s s the imereial e (Pinus or sugar metimes be Pinus at 60 to ) it shall 0 5% all weigh Mote 1.) D358 9, Character of Wood 9.1 The wood shall be free of knots, pitch pockets, and other defects. The color of the wood shall be uniform across each panel with no streaks that are excessively light or dark, the number ofannual growth rings per inch along the radius ofthe log from which the wood was obtained shall be not less tlian 15. The surfaces shall be smoothly planed and sanded thoroughly with 150 grit sandpaper within two weeks of testing. 9.2 The wood shall be selected as edge grain or flat grain as desired. The test surface of flat grain wood shall be on the bark side. 10. Thickness of Panels 10.1 The minimum thicknesses (see Note 3) in proportion w width (across the grain) shall be as follows: Panel Width, in. (mm) Minimum Thickness, in. (mm) Less than 3 (less than 7S) 3 to 6 (75 to 150) Over 6 (over ISO) SOUTHERN PINE Vi6 (11) Vis (It) % (19) tl. Species 11.1 The material for test panels shall be southern pine {Pinus sp.), suitable for siding purposes. It is not to be limited to a single species, but shall conform to the require ments prescribed in Sections 12 and 13. 12. Weight per Volume 12.1 When the wood is in equilibrium with air at .60 to 65 % relative humidity and 70 IT (21 0.5`C) it shall jreigh 32 to 38 lb/ft3 (510 to 610 kg/m3) or at 50 5 % relative humidity and 73.5 3.5F (23 2C) it shall weigh 31 to 37 lb/ft3 (500 590 kg/m3). (See Note 2.) 13. Character of Wood 13.1 The wood shall be free of knots, pitch pockets, and other defects. The color of the wood shall be uniform across each panel with no streaks that are excessively light or dark. The number ofannual growth rings per inch along the radius ofthe log from which the wood was obtained shall be not less than 4 nor more than 12. The surfaces shall be smoothly planed and sanded thoroughly with 150 grit sandpaper within two weeks of testing. 13.2 The wood shall be sapwood having flat grain. 14. Thickness of Panels 14.1 The minimum thicknesses (see Note 3) in proportion to width (across the grain) shall be as follows: Panel Width, in. (mm) Minimum Thickness, in, (mm) Less than 3 (less than 75) 3to 6 (75 to 150) Over 6 (over 150) Vis (11) Vis (It) %(19) REDWOOD 15. Species 15.1 The material for test panels shall be redwood (Sequoia sempervirens). 16. Weight per Volume 16.1 When the wood is in equilibrium with air at 60 to 65 % relative humidity and 70 IT (21 0.5C) it shall weigh 28 to 29 lb/ft3 (450 to 460 kg/m3) or at 50 5 % relative humidity and 73.5 3.5F (23 2C) it shall weigh 27.2 to 28.2 lb/ft3 (436 to 452 kg/m3). (See Note 1.) 17. Character of Wood 17.1 The material shall be heartwood, as nearly edge grain as possible. The number of annual growth rings per inch along the radius of the log from which the wood was obtained shall be not less than 18. The wood shall be free of knots, oil streaks, and other defects such as wavy burl grain. The color of the wood shall be uniform across each panel with no streaks that are excessively light or dark. The surfaces shall be smoothly planed and sanded thoroughly with 150 grit sandpaper within two weeks of testing. 18. Thickness of Panels 18.1 The minimum thicknesses (see Note 2) in proportion to width (across the grain) shall be as follows: Panel Width, in. (mm) Less than 3 (less than 75) 3 to 6 (75 to 150) Over 6 (over 150) Minimum Thickness, in. (mm) Vs (10) '/us (11) % (19) DOUGLAS FIR 19. Species 19.1 The material for test panels shall be Douglas fir {Pseudotsuga menziesii). 20. Weight per Volume 20.1 When the wood is in equilibrium with air at 60 to 65 % relative humidity and 70 IT (21 0.5C) it shall weigh 30 36 lb/ft3 (480 to 580 kg/m3) or at 50 5 % relative humidity and 73.5 3.5T (23 2C) it shall weigh 29 to 35 lb/ft3 (460 to 560 kg/m3). (See Note 1.) 21. Character of Wood 21.1 The wood shall be free of knots, pitch pockets, and other defects. The color of the wood shall be uniform across each panel with no streaks that are excessively light or dark. The number of annual growth rings per inch along the radius ofthe log from which the wood was obtained shall be not less than ten. The surfaces shall be smoothly planed and sanded thoroughly with 150 grit sandpaper within two weeks of testing. 21.2 The wood shall be heartwood and selected as edge grain or flat grain as desired. The test surface of flat grain wood shall be on the bark side. 22. Thickness of Panels 22.1 The minimum thicknesses (see Note 2) in proportion to width (across the grain) shall be as follows: Panel Width, in. (mm) Minimum Thickness, in. (mm) Less than 3 (less than. 75) 3 to 6 (75 to 150) Over 6 (over 150) (11) Vi6(U) 3A (19) 45 DUP050297228 <) D 358 The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. Scope 1.1 T1 resistanC' ings on s 1.2 7/ ations, c. address < the resp> appropri. applicab 2. Refer 2.1 A. D823 Thit Test D 100 Thit D 118Dry to a D140Dr> piie 3. Sumi 3.1 T form tb materia! over a n is detent over a c< are bent 4. Signi 4.1 C substratt l; when th DUP050297229 dji m Designation: D 522 - 88e1 Standard Test Methods for Mandrel Bend Test of Attached Organic Coatings1 This standard is issued under the fixed designation D 522; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department of Defense to replace Method 6222 of Federal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. l No t e--Table 2 was editorially corrected in May 1989. 1. Scope 1.1 These test methods cover the determination of the resistance to cracking (flexibility) of attached organic coat ings on substrates of sheet metal or rubber-type materials. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 3. Summary of Test Methods 3.1 The coating materials under test are applied at uni form thickness to panels of sheet metal or rubber-type materials. After drying or curing the coated panels are bent over a mandrel and the resistance to cracking of the coating is determined. In Test Method A the coated panels are bent over a conical mandrel. In Test Method B the coated panels are bent over cylindrical mandrels of various diameters. 4. Significance and Use 4.1 Coatings attached to substrates are elongated when the substrates are bent during the manufacture of articles or when the articles are abused in service. These test methods These test methods are under the jurisdiction of ASTM Committee D-l on Is' and Related Coatings and Materials and is the direct responsibility of "rcommittee DO 1.23 on Physical Properties of Applied Paint Films. Current edition approved May 27,1988. Published November 1988. Originally Wnished as D 522 - 39. Last previous edition D 522 - 85. 'Annual Book ofASTM Standards, Vol 06.01. have been useful in rating attached coatings for their ability to resist cracking when elongated. They have been useful in evaluating the flexibility of coatings on flexible substrates. 5. Test Specimens 5.1 Substrates: 5.1.1 If the purpose of the test is to determine the percent of elongation of the coating material, the substrate shall be cold-rolled steel strip V32 in. (0.8 mm) (22 gage) thick. 5.1.2 If the purpose of the test is to rate the coated material for resistance to cracking, the substrate may be any type of sheet metal or rubber-type material (for example, steel, aluminum, tinplate, or synthetic rubber). The thickness of the sheet metal may be less than V32 in. (0.8 mm) and the thickness of the rubber-type materials may be as great as V2 in. (13 mm). 5.1.3 The recommended panel size is 4 in. (100 mm) in width and 6 in. (150 mm) in length. The maximum size that the conical mandrel can accommodate is 4Vi in, (115 mm) wide and 7 Vi in. (190 mm) long. 5.1.4 The. surface preparation of the substrate shall be agreed upon between the purchaser and the seller. Prior to the application of the coating, round slightly the edges of metal panels to remove burrs in order to eliminate anoma lous edge effects. No t e 1--If elongations are to be determined for coatings applied to substrates other than V32 in. (0.8 mm) thick cold-rolled steel, they must be measured with a special mandrel jig as described in Appendix Xl.2 and shown in Fig. X1.1. The procedure for using the jig is described in Appendix XI.3. 5.2 Coated Panels: 5.2.1 Apply uniform coatings of the materials under test to the substrates in accordance with Test Methods D 823 and air dry or bake under conditions mutually agreeable to the purchaser and the seller. If percent elongation is to be measured, a minimum thickness of 1.0 mil is required on V32 in. (0.8 mm) thick cold-rolled steel. Perform a minimum of three determinations of coating thickness on each of the specimens in accordance with Test Methods D1005, D 1186, or D 1400. 6. Conditioning and Number of Tests 6.1 Condition the test specimens for at least 24 h at 73.5 3.5F (23 2C) and 50 5 % relative humidity, and test in the same environment or immediately on removal therefrom 47 DUP0502 97230 # D 522 unless otherwise specified by the purchaser and seller. 6.2 Test at least three replicate specimens in Test Method A and at least two replicate specimens in Test Method B at each mandrel diameter of interest. TEST METHOD A--CONICAL MANDREL TEST 7. Apparatus 7.1 Conical Mandrel Tester, consisting of a metal cone, a rotating panel-bending arm. and panel clamps, all mounted on a metal base as illustrated in Fig. I. 7.1.1 Cone, smooth steel, 8 in. (203 mm) in length, with a diameter of Vs in. (3 mm) at one end and a diameter of 1V2 in. (38 mm) at the other end. 8. Procedure 8.1 With the operating lever of the apparatus in a hori zontal position, slip the test specimen between the mandrel and the drawbar with the finish side towards the drawbar. Rigidly clamp the specimen in a vertical position adjacent to the mandrel by placing the long edge behind the clamping bar in such a manner that the panel is always set up to the narrow end of the mandrel. Slip two sheets of No. 1 brown kraft wrapping paper, substrate 30, thoroughly lubricated on each side with talc, between the specimen and the drawbar and hold in position only by the pressure of the drawbar against the paper. 8.2 Move the lever through about 180 at uniform ve locity to bend the specimen approximately 135, If the purpose ofthe test is to measure percent elongation, the bend time should be about 15 s. To determine crack resistance under more simulated use conditions, the bend time should be some value between 1.5 s and 5 s to be agreed upon between the purchaser and the seller. 8.3 Examine the bent surface of the specimen immedi ately with the unaided eye for cracking. Having determined and suitably marked the end of the crack farthest from the small end of the mandrel, which shall be considered as the end point, bring the drawbar to the starting position and remove the panel from the mandrel. Measure the distance from the farthest end of the crack to the small end of the mandrel. This distance is used to compute the elongation. The mandrel diameter at which cracking ceased is taken as the resistance to cracking value. N' 2--In some cases, the measured distance is used as a measure of crack resistance. 9. Calculation 9.1 Determine the elongation of the finish from the plotted curve in Fig. 2. This curve represents the relationship between the percent elongation and the diameter of the conical mandrel for a 1.0 mil coating thickness. The relation between the distance along the conical mandrel and the corresponding diameter has also been plotted on this curve 9.2 Adjust the percent elongation value obtained from Fig. 2 for coating thickness by adding the correction obtained from Fig. 3. i ^ I ; | No t e 3--Example--Suppose a visual examination of the finish on the bent cold-relied steel specimens Vn in. (0.8 mm) in thickness shows that the end of the first crack in the coating is at a distance of 3 in. (75 mm) from the small end of the cone. From Fig. 2 determine the percem elongation of the film from the measured crack distance, in this example 5.2 %. To correct for coating thickness add the value obtained in Fig. 3 At a crack distance of 3 in. the correction per mil (25 pm) of coating thickness is 0.3 %. If the film thickness in the example is 2 mils (50 pad the actual percem elongation is 5.2 + (2 x 0.3) = 5.8 %. I 10. Report 10.1 Report the following information: 10.1.1 Mean and range of coating elongation or resistance to cracking values for each specimen, 10.1.2 Mean and range of coating film thickness for each specimen, | 10.1.3 Specimen preparation proceduresused, 1 10.1.4 Test conditions, and 1 10.1.5 Mean and range of elongation or resistance to f cracking, and film thickness for thereplicatespecimens. 1 12. 1 sur mn in. An in I 13. 1 unc r ove fmg mai beii Rer visi repi 11. Precision 11.1 Results are not available to determine the precision of this test method. This test method has been in use for many years and is considered acceptable for evaluating theresistance to cracking of attached coatings. FIG. 1 Conical Mandrel Test Apparatus s S / t / / Ou COLD ROLLED STEEL \ ;A :s : Ji! 1E0L01N28A1T4I0H18IN 1P8ER20CE2N2T 2 4 2 8 28 30 32* FIG. 2 Distance Along Cone and Corresponding Mandrel Sftfjj versus Percent Elongation for Specimens on Cold-Rolled Steel in. (0.8 mm) in Thickness 48 L DUP050297231 :n as ;asure the iship f the ation i the urve. from lined ish on shows in. (75 ercent ample Fig. 3. oating 0 pm). itance : each ice to is. CORRECTION TO RE ADDED TO PER-CEHT EL0N9ATI0N FIG. 3 Correction for Thickness of Film TEST METHOD B--CYLINDRICAL MANDREL TEST 12. Apparatus 12.1 Elongation Test Equipment, consisting of rods or surfaces, including cylindrical steel diameters of 1 in. (25 mm), % in. (19 mm), Vi in. (12.7 mm), 3/s in. (9.5 mm), 'A in. (6.4 mm), and Vs in. (3.2 mm), mounted on a metal base. An example of an acceptable form of this device is illustrated in Fig. 4. 13. Procedure 13.1 Place the test panel over a mandrel with the uncoated side in contact and with at least 2 in. (50 mm) overhang on either side. Using a steady pressure of the fingers, bend the panel approximately 180 around the mandrel at a uniform velocity in a time of 1.5 to 5 s, the time being that agreed upon between the purchaser and the seller. Remove and examine the panel immediately for cracking visible to the unaided eye. If cracking has not occurred, repeat the procedure using successively smaller diameter mandrels on previously untested areas of a specimen until failure occurs or until the smallest diameter mandrel has been used. ' 13.1.1 This procedure can be applied as a "pass/fail" test by determining whether cracking is produced by a specified mandrel size. 13.1.2 The resistance to cracking value for a coating is taken as the mandrel diameter at which cracking ceases. 14. Calculation 14.1 Determine the elongation range of the material from Table 1 in which the elongation of a I mil (25 pm) thick coating on 1/32 in. (0.8 mm) cold-rolled steel is given for each mandrel diameter. 14.2 If the coating thickness exceeds 1 mil (25 pm), correct the determined elongation for film thickness using the factors for each mandrel diameter given in Table 2. Calculate the total elongation of the coating as follows: E -- e, + ic, where: E -- total elongation, %, Ci = elongation from Table 1, %, t = thickness, mils, and Ci = correction factor from Table 2. 15. Report 15.1 Report the following information: TABLE 1 Manor?! Diameter, in. (mm) 1 '25) %M9) W (12.7) % (9.5) Va {6.4) Vi (3.2) Elongation Elongation, % 3.3 4.4 6.75 9.0 14.0 28.0 TABLE 2 Correction lor Rim Thickness Mandrel Diameter, in. (mm) Correction Factor 1 125) 3/x (19) W (12.7) ;Ve (9.5) V,. (3.4) ' Vi. (3.2) 0.21 0.26 0.38 0.50 0.71 1.40 DUP0502 97232 0 522 15.1.1 Mean and range of coating elongation or resistance to cracking values for each specimen, 15.1.2 Mean and range of coating thickness for each specimen, 15.1.3 Specimen preparation procedures used, 15.1.4 Test conditions, and 15.1.5 Mean and range of elongation, resistance to cracking, and film thickness for the replicate specimens. 16. Precision and Bias 16.1 Results are not available to determine the precision of these test methods. These test methods have been in use for many years and are considered acceptable for evaluating the crack resistance of attached coatings. INDEX TERMS 17. Index Terms 17.1 These test methods are indexed under the following terms: cracking; flexibility; resistance--cracking. APPENDIX (Nonmandatory Information) I XI. RELATIONSHIP BETWEEN ELONGATION AND MANDREL SIZE Xl.l In the mandrel test, the specimens are elongated considerably past their elastic limit. Therefore, the elonga tions obtained are considerably higher than elongation values calculated from a theoretical equation that is based on the assumption that the elastic limits of the specimens are not exceeded. X1.2 The elongation values corresponding to mandrel diameters in Figs. 2 and 3 of these test methods were obtained by direct measurements with a special mandrel jig. X1.3 This jig shown in Fig. Xl.l consists of two forks for holding the mandrel and specimen in position and a roller with which the specimen is tightly wrapped around and held against the mandrel. X1.4 Measuring Elongation With Jig--Make two parallel gage scratches with a sharp stylus on the edge of the specimen so located that when it is wrapped around the mandrel the included angle between the scratches will be approximately 180. In locating the scratches, it is necessary to make sure that they will be within the section of the specimen that, after bending, is tightly wrapped against the mandrel. Having located the scratches, measure the linear distance between them to within 2 pm. Clamp the specimen in the jig and bring the roller down tight against it. Draw the roller around causing the specimen to be tightly wrapped and secured against the surface of the mandrel. In order to hold the jig in this position hold the forks together with a C-clamp. Then rigidly mount the clamped jig on the table of the measuring machine.3 Each of the gage scratches shall hemade to coincide with the vertical cross-hair of the mea suring eyeuiece while the horizontal cross-hair is tangent to the curvature of the upper surface of the specimen. Take the angle read! o r at each of these points. The difference between the two angie readings is a measure of the included angle formed by the two gage scratches, and the radii drawn coincident with the scratches. Read the angle readings in minutes and seconds to a precision of5 s. Also determine the total diameter of the mandrel and the bent specimen. From these data calculate the percent elongation E at the surface of the specimen as follows: L - a7r/180r =[(.- d)/d] x 100 where: = angle, = arc = rad hr thief: = orb'd f urvature for system (mandrel radius + + coating thickness), and 'stance between scratches. 3 A star..........has been found suitable for this purpose. 50 DUF050297233 i use iting wing # D 522 The American Society for Testing andMaterials takes noposition respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision atany time by the responsible technical committee and must be reviewed every five years and If not revised, either reepproved or withdrawn. Yourcomments are invited either for revision of this standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ' the I the II be ssary ' the t the near men vthe land hold th a 'le of J1 be mea nt to ethe ween ingle *awn s in the rom of )anel 51 DUP050297234 Designation: D 523 - 89 Standard Test Method for Specular Gloss1 TABLE This standard is issued under the fixed designation D 523; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This lest method has been approvedfor use by agencies of the Department of Defense. Consult the DoD Index ofSpecifications and Standardsfor the specific year of issue which has been adopted by the Department of Defense. 1. Scope 1.1 This test method covers the measurement of the specular gloss of nonmetallic specimens for glossmeter geom etries of 60, 20, and 85 (1-7).2 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address ail ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D3964 Practice for Selection of Coating Specimens for Appearance Measurements3 D3980 Practice for Interlaboratory Testing of Paint and Related Materials3 D4039 Test Method for Reflection Haze of High-Gloss Surfaces4 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry5 E 430 Method for Measurement of Gloss of High-Gloss Surfaces by Goniophotometry5 3. Terminology 3.1 Definitions: 3.1.1 relative luminous reflectance factor--the ratio of the luminous flux reflected from a specimen to the luminous flux reflected from a standard surface under the same geometric conditions. For the purpose of measuring specular gloss, the standard surface is polished glass. 3.1.2 specular gloss--the relative luminous reflectance factor of a specimen in the mirror direction. 4. Summary of Test Method 4.1 Measurements are made with 60, 20, or 85 geometry 1 This test method is under the jurisdiction of ASTM Committee D-l on Faint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.26 on Optical Properties. Current edition approved March 31, 1989. Published May 1989. Originally published as D 523 - 39 T. Last previous edition D 523 - 85l. 2 The boldface numbers in parentheses refer to the list of references at the end of this test method. 3 Annua! Book ofASTM Standards, Vol 06.01. * Annual Book ofASTM Standards, Vol$06.0! and 06.02. 5 Annual Book ofASTM Standards, Vols 6.01 and 14.02. (8,9). The geometry of angles and apertures is chosen so that these procedures may be used as follows: 4.1.1 The 60 geometry is used for intercomparing most specimens and for determining when the 20 geometry may be more applicable. 4.1.2 The 20 geometry is advantageous for comparing specimens having 60 gloss values higher than 70. 4.1.3 The 85 geometry is used for comparing specimens for sheen or near-grazing shininess. It is most frequently applied when specimens have 60gloss values lower than 10, 5. Significance and Use 5.1 Gloss is associated with the capacity of a surface to reflect more light in some directions than in others. The directions associated with mirror (or specular) reflection normally have the highest reflectances. Measurements by this test method correlate with visual observations of surface shininess made at roughly the corresponding angles. 5.1.1 Measured gloss ratings by this test method arc obtained by comparing the specular reflectance from the specimen to that from a black glass standard. Since specular reflectance depends also on the surface refractive index ofthe specimen, the measured gloss ratings change as the surface refractive index changes. In obtaining the visual gloss ratings, however, it is customary to compare the specular reflectances of two specimens having similar surface refractive indices. Since the instrumental ratings are affected more than the visual ratings by changes in surface refractive index, non agreement bet--.vp.en visual and instrumental gloss ratings can occur when mb: gloss specimen surfaces differing in refrac tive index me compared. 5.2 Other vis-'si aspects of surface appearance, such as distinctness cl reflected images, reflection haze, and texture; are freque; t iy i r.volved in the assessment ofgloss (1), (6), (1) Method E 430 in dudes techniques for the measurement of both distinctness - of-image gloss and reflection haze. Test Method O "039 - tovides an alternative procedure for nx* suring n mze. 5.3 Little information about the relation of numerical to-percer>t"n! intervals of specular gloss has been publishei However cmmy applications the gloss scales of this test method It provided discriminations between coated spec- imens tin m agreed well with visual discriminations a gloss (!' 5.4 V I mens differing widely in perceived gloss a j color, or compared, nonlinearity may be encous- tered in emship between visual gloss different ratings a enta! gloss reading differences. Tolerar gO0 recep Tolerar 20" recep Tolerar 85" recep Toleran 6. App: 6.1 1 sist of; beam, r teceptoi reflected sitive dt 6.2 6 shall be to the s} the min axis of tl within 0 With a f mirror ii be formi window) shall be center ol and tolei in Table are mer beam-ty 6 A list Headquaru 52 DUP050297235 iothat ; most y may paring imens uently an 10. ace to s. The ection nts by surface >d are m the tecular of the .urface atings, :tances ndices. \n the non*s can efrac- ch as xture, 6), (7). lent of j. Test r mea- lericalilished. his test d specions of lloss or ncoun-, Terence D 523 TABLE 1 Angles and Relative Dimensions oi Source Image and Receptors In Plane of Measurement Perpendicular to Plane of Measurement , 2 tan 9/2 Relative Dimension 9, 2 tan 9/2 Relative Dimension Source image 0.75 0.0131 Tolerance 0.25 0.0044 0.171 0.057 2.5 0.0436 0.5 0.0087 0.568 0.114 60 receptor 4.4 Tolerance 0.1 0.0768 0.0018 1.000 0.023 11.7 0.2049 0.2 0.0035 2.668 0.046 20 receptor 1.8 0.0314 Tolerance 0.05 0.0009 0.409 0.012 3.6 0.0629 0.1 0.0018 0.819 0.023 06 receptor 4.0 Tolerance 0.3 0.0698 0.0052 0.909 0.068 6.0 0.1048 0.3 0.0052 1.365 0.068 6, Apparatus6 6.1 Instrumental Components--The apparatus shall con sist of an incandescent light source furnishing an incident means for locating the surface of the specimen, and a receptor located to receive the required pyramid of rays reflected by the specimen. The receptor shall be a photosen sitive device responding to visible radiation. 6.2 Geometric Conditions--The axis of the incident beam shall be at one of the specified angles from the perpendicular to the specimen surface. The axis of the receptor shall be at the mirror reflection of the axis of the incident beam. The axis of the incident beam and the axis ofthe receptor shall be within 0.1* of the nominal value indicated by the geometry. With a flat piece ofpolished black glass or other front-surface mirror in the specimen position, an image ofthe source shall be formed at the center of the receptor field stop (receptor window). The length of the illuminated area of the specimen shall be not more than one third of the distance from the center of this area to the receptor field stop. The dimensions and tolerance ofthe source and receptor shall be as indicated in Table 1. The angular dimensions of the receptor field stop are measured from the receptor lens in a collimatedbeam-type instrument, as illustrated in Fig. 1, and from the 6 A list of manufacturers of glossmeters can be obtained from ASTM Headquarters. test surface in a converging-beam-type instrument, as illus trated in Fig. 2. See Figs. 1 and 2 for a generalized illustration of the dimensions. The tolerances are chosen so that errors in the son rce and receptor apertures do not produce an error of more ilia a one gloss unit at any point on the scale (5). 6.2.1 The important geometric dimensions of any specular-gloss measurement are: 6.2.1.1 Beam axis angle(s), usually 60, 20, or 85. 6.2.1.2 Accepted angular divergences from principal rays (degree of spreading or diffusion of the reflected beam). N' I--The parallel-beam glossmeters possess the better unifor mity of principle-ray angle of reflection, but the converging-beam glossmeters possess the better uniformity in extent of angular divergence accepted for measurement No t )- tarization--An evaluation of the impact of polarization on I rement has been reported (11). The magnitude of the polari?.;. ind: e: ; or depends on the difference between the refractive n and standard, the angle of incidence, and the degree of i'.'dr . because the specimen and standard are generally quite sirr * i ` measured gloss values are little affected by polariza tion. 6. ' vng--There shall be no vignetting of rays that lie '" ' "ield angles specified in Table 1. 6 ` ... - " Conditions--Results should not differ signif icant / fret those obtained with a source-filter photocell con ' a;' ;i that is spectrally corrected to yield CIE lumi- no- '- ". ' y with CIE source C. Since specular reflection is, ia ; ), spectrally nonselective, spectral corrections need t > r applied only to highly chromatic, low-gloss sperir ' n agreement of users of this test method. 6.5 "mem Mechanism--The receptor-measure- m ^hall give a numerical indication that is prr; c r> the, light flux passing the receptor field stop wiri ' a f full-scale reading. 7. Iv:5 -T-e Standards 7.1 glas; she ' geo indot siris a I '. Standards--Highly polished, plane, black Tractive index of 1.567 for the sodium D line c ; d a specular gloss value of 100 for each gloss value for glass of any other refractive computed from the Fresnel equation (5). For ces in refractive index, however, the gloss value .ction of index, but the rate of change of gloss FIG. 1 Diagram ol Parallel-Beam Glossmeter Showing o 53 s - rce Mirror-Image Position DUP050297236 # D 523 TEST SPECIMEN su CO vi< in co sp by pe tu tb< in I with index is different for each geometry. Each 0.001 increment in refractive index produces a change of 0.27, 0.16, and 0.016 in the gloss value assigned to a polished standard for the 20,60, and 85geometries, respectively. For example, glass of index 1.527 would be assigned values of 89.2, 93.6, and 99.4, in order of increasing geometry. N' 3--Polished black glass has been reported to change in refractive index with time largely due to chemical contamination (10). The original values can be restored by optical polishing with cerium oxide. A wedge of high-purity quartz provides a more stable reference standard than glass. 7.2 Working Standards1--Ceramic tile, depolished ground opaque glass, emery paper, and other semigloss materials having hard and uniform surfaces are suitable when calibrated against a primary standard on a glossmeter known to meet the requirements of this test method. Such standards should be checked periodically for constancy by comparing with primary standards. 7.3 Store standards in a closed container when not in use. Keep them clean and away from any dirt that might scratch or mar their surfaces. Never place standards face down on a surface that may be dirty or abrasive. Always hold standards at the side edges to avoid getting oil from the skin on the standard surface. Clean the standards in warm water and a mild detergent solution brushing gently with a soft nylon brush. (Do not use soap solutions to clean standards, because they can leave a film.) Rinse standards in hot running water (temperature near 150F (65C)) to remove detergent solu tion, followed by a final rinse in distilled water. Do not wipe standards. The polished black glass high-gloss standard may be dabbed gently with a lint-free paper towel or other lint-free absorbent material. Place the rinsed standards in a warm oven to dry. 8. Preparation and Selection of Test Specimens 8.1 This test method does not cover preparation tech niques. Whenever a test for gloss requires the preparation of test specimens, use the procedures given in Test Methods D823. 7 Gloss standards are available from Byk/Gardner, 2435 Linden Lane, Silver Spring, MD 20910 and Hunter Associates Laboratory, Inc., 11495 Sunset Hills Road, Reston, VA 22090. I No r;: 4--To determine the maximum gloss obtainable from a teg maten;as a paint or varnish, use Methods B or C of Teg Methods ); 8.2 ; 3 t specimens in accordance with Practice D 394_ 9. Iii.sT :;; - Calibration 9.10 ; the glossmeter in accordance with the tnanufactui'd .O: Tractions. 9.2 -he instrument zero by placing a black cavity ij the si. : . position. If the reading is not within 0.1 of zero, t it algebraically from subsequent readings or adjust ; . Tirument to read zero. 92 ' the instrument at the start and completion of e .id of glossmeter operation, and during the opto - TCCntly frequent intervals to assure that the instr- onse is practically constant. To calibrate, adjt ament to read correctly the gloss of a highly pels 1 rl, properly positioned and oriented, and' the: , o dioss of a working standard in the mid-gloss ra; " no( > orarnent reading for the second standard does :n one unit of its assigned values, check' cl i repeat. If the instrument reading fortKf sec d still does not agree within one unit ofitf asst-, repeat with another mid-range standard. If the *. still more than one unit, do not use tht in, oboe readjustment, preferably by the mana- far, 10. 'each specimen in turn beneath (or on) the gf specimens with brush marks or similar te, r' -' <:. them in such a way that the directions o' ullel to the plane of the axes of lte| inc- a fleeted beams. t three readings on a 3 by 6-in. (75 bf : test specimen. If the range is gaMS| tlv- , take additional readings and calcuhta the rding divergent results as in the sectiotf|p CP s of Practice D 3980. For larger sped" m: i'o : tionateiy greater number of readings. 1J don di -bse corrections only upon agreement twr ' ' and the user. To apply the correct! 12 us< of tin ne prt glc 13 lab dif fer rat foi de' thi sir (2) 54 DUP050297237 om a test - of Test D 3964. e manu- cavity in 0.1 of dings or mpletion tring the : that the :alibrate. a highly ted, and nid-gloss lard does :s, check > for the ait of its idard. If use the j manu- ir on) the r similar directions es of the i by ement be:orrection' w. CM Subtract it from the glossmeter reading. To measure the correction, illuminate the specimen perpendicularly and view at the incident angle with the receiver aperture specified in 6.2 for the corresponding geometry. To compute the correction, multiply the 45, 0 directional reflectance of the specimen, determined in accordance with Test Method E 97, by the effective fraction of the luminous flux reflected by the perfect diffuse reflector and accepted by the receiver aper ture. The luminous flux entering the receiver aperture from the perfect white diffusor would give the following gloss indications for each of the geometries: Geometry, * Gloss of Perfect White Diffuser 60 2.5 20 1.2 85 0.03 12. Report 12.1 Report the information following: 12.1.1 Mean specular gloss readings and the geometry used. 12.1.2 If uniformity of surface is of interest, the presence ofany specimen that exhibits gloss readings varying by more than 5 % from their mean. 12.1.3 Where preparation of the test specimen has been necessary, a description or identification of the method of preparation. 12.1.4 Manufacturer's name and model designation ofthe glossmeter. 12.1.5 Working standard or standards of gloss used. 13. Precision 13.1 On the basis of studies of this test method by several laboratories in which single determinations were made on different days on several ceramic tiles and painted panels dif fering in visually perceived gloss, the pooled within-laboratory and between-laboratories standard deviations were found to be those shown in Table 2. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 13.1.1 Repeatability--Two results, each of which are angle determinations obtained on the same specimen by the Ty r- G 2!.' G A SW e Hot rr : san me Tab: e It thn diff difi' give: pree n N: mem con;; be pn n Standard Deviation of Gloss Determinations ;o. of r'Oinic :es 4 4 2 Degrees of Freedom Within- BetweenLabora- Labora- tory tories 40 34 40 34 16 6 3. Of bated aiels Degrees of Freedom WithinLabora tory BetweenLabora tories 8 80 72 '12 220 136 5 48 18 YaUvns. Yiree determinations. Standard Deviations WithinLaboratory* 0.4 0.3 0.2 BetweenLaboratories 1.2 1.2 0.6 Standard Deviations WithinLabora tory'1 0.6 0.3 0.3 BetweenLabora tories 2.2 1.2 2.4 : num Acceptable Differences for Two Results Repeatability (Within Laboratories)4 Ceramic "I'ies Painted Panels 1.1 1.7 0.9 0.9 0.6 0.8 Reproducibility (Between Laboratories)8 Ceramic Tiles 3.5 3.4 2.0 Painted Panels 6.4 3.5 7.2 'nations. ::-ee determinations. should be considered suspect if they differ by r.iaximum acceptable differences given in -.inability--Two results, each the mean of : ions, obtained on the same specimen by nr.cries should be considered suspect if they .u the maximum acceptable differences This does not include variability due to n els in different laboratories. e types of paint, particularly semi-gloss, the cted by method of film preparation and drying reproducibility of results from such materials may . alues given in Table 3. REFERENCE:: (I) Hunter, R. S., "Methods of Determining Gloss," Proceedings, ASTM, Vol 36, 1936, Part II, p. 783. Also, Journal of Research, Nat. Bureau Standards, Vol 18, No. 1, January 1937, p. 19 {Research Paper RP958). Six somewhat different appearance attributes are shown to be variously associated with gloss. There- fore, as many as six different photometric scales may be required to handle all gloss measurement problems. (This paper is out of print). ffl Hunter, R. S-, and Judd, D. B., "Development of a Method of Gassifying Paint According to Gloss," ASTM Bulletin, No. 97, March 1939, p. 11. A comparison is made ofseveral geometrically different photometric scales for separating paint finishes for gloss. The geometric conditions of test later incorporated in Test Method D 523 are recommended. (3) Wetlaufer, L. A., and Scott, W. E,, "The Measurement of Gloss," industrial and Engineering Chemistry, Analytical Edition, Vol 12, November 1940, p. 647. A goniophotometric study of a number of Paint finishes illuminated at 45; a study of gloss readings affected (4) <5; : r sy u ' (6) (7) ! 55 noerture for 45 and 60 incidence. he Gloss Measurement ofFaint Finishes," ASTM : j b January 1948, p. 72. History of Test Method ;C, III, and Nimerroff, I., "Measurement of . :uiar Gloss," Journal of Research, Nat. Bureau " y of the effect of aperture variation on glossmeter e g definitions of terms used in connection with suienwm, the Fresnel equation in a form readily .ration, and the deviation of diffuse correction Gloss Evaluation of Materials," ASTM Bulletin, anher 1952, p. 48. A study of the history of gloss hf and other societies, describing the background' eometry of these methods. Contains photographs eisaracteristics of a variety of methods. The Measurement of Appearance, WileyYo: k, 1975, Chapter 6, "Scales for Gloss and DUP050297238 D 523 OtherGeometric Attributes," and Chapter 13, "Instruments for the Geometric Attributes of Object Appearance." (8) Homing, S. C., and Morse, M. P., "Measurement of the Gloss of Paint Panels," Official Digest, Federation of Paint and Varnish Production Clubs, March 1947, p. 153. A study of the effect of geometric conditions on results of gloss tests with special attention to high-gloss panels. (9) Huey, S,, Hunter, R. S., Schreckendgust, J. G,, and Hammond, H. K., Ill, "Symposium on Gloss Measurement," Official Digest, Vol 36, No. 471, April 1964, p. 343. Contains discussion of industrial experience in measurement of 60 specular gloss (Huey), high-gloss measure. : r sheen sv; as glosser.:- : (10) Bilim.and tvlr ,t. Coloi i, t Compa ments series <.. anal\7. i (11) Budde, \'..' qfComii h i . filiation of low-gloss finishes with 85" i;.chreckendgust), and gloss standards and aia (Hammond). n-onneil, F. X. D., "Visual Gloss Scaling . ''mg Analysis of Painted Specimens," ipLcatiom, Vot 12, 1987, pp 315-326. ' ratings with instrumental measure- nctness of image gloss, and haze for - hire painted specimens. The data are r.-.crrinnal scaling. Ions in Gloss Measurements," Journal '1 52, June 1980, pp. 44-48. The American Society for Testing and Materials takes no position respecting the vs with any item mentioned in this standard. Users of this standard are expressly advi.v i patent rights, and the risk of infringement of such rights, are entirely their own respo This standard is subject to revision at any time by the responsible technical. o ifnotrevised, eitherreapproved or withdrawn. Your comments are Invited eithc and should be addressed to ASTM Headquarters. Your comments will rece.i technical committee, which you may attend. It you feel that your comments; views known to the ASTM Committee on Standards, 1916 Race St., Phiiade'p rights asserted In connection - of the validity of any such id every five years and additional standards g of the responsible u should make your 1. Sc 1.! consi viscoi 1.2 probh whom i priate bility | 2. Re 2.1 E1 3. Tei 3.1 3.1. freque 3.1.. to exp brush produt 4. Sui 4.1 of 200 detern 5. Sig 5.1 specify consun 6- App 6.1 ) illustrai ? ment it without 56 DUP0502 97239 Designation: D 562 - 81 (Reapproved 1990)1 Standard Test Method for Consistency of Paints Using the Sf r This standard is issued under the fixed designation D562; the number im: j c original adoption or, in the case of revision, the year of last revision. An superscript epsilon (e) indicates an editorial change since the last revision : t This method has been approved for use by agencies of the Departmen Standards for the specific year of issue which has been adopted by the D. 61 No t e--Editorial changes were made throughout in May 1990. ameter1 . lie designation indicates the year of . $ >$ indicates the year of last reapproval. A me OoD Index of Specifications and .. . 1. Scope 1.1 This test method covers the determination of the consistency of paints and related coatings using the Stormer viscometer. 1.2 This standard does not purport to address the safety probiems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: E 1 Specification for ASTM Thermometers2 3. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 consistency--load in grams to produce a rotational frequency of 200 r/min. 3.1.2 Krebs units (KU)--values of a scale commonly used to express the consistency of paints generally applied by brush or roller. This scale is a log function of the "load to produce 200-r/min" scale. strob' ~.cv 6.' 61 eter. 7 nv - the * ..... . . 7. o' 7 (poise , be ST: ;S: p. No t : ; viscocTes ; I.'.' see-, .. 4. Summary of Test Method 4.1 The load required to produce a rotational frequency of200 r/min for an offset paddle rotor immersed in a paint is determined. 5. Significance and Use 5.1 This test method provides values that are useful in specifying and controlling the consistency of paints, such as consumer or trade sales products. 6. Apparatus 6.1 Viscometer,3 Stormer, with the paddle-type rotor as illustrated in Figs. 1 and 2. The stroboscopic timer attach ment in Fig. 1 can be removed and the instrument used without it but with a sacrifice of speed and accuracy. The ; vb v- P g V: ` ......... sa 1' This test method is under the jurisdiction of ASTM Committee D-l on Paint *(d Related Coatings and Materials and is the direct responsibility of SubcomB|ttee D01.24 on Physical Properties of Liquid Paints and Paint Materials. Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 562 - 47 T. Last previous edition D 562 - 55 (1976). Annual Book ofASTM Standards. Vols 05.03 and 14.01. O. Ei V:s- 7J.:< ! K/cVJ . . 57 ' : \ es the 200 r/min reading directly. : -1 (500-mL), 33/s in. (85 mm) in diam- A.n ASTM Stormer Viscosity therfrom 20 to 70C and conforming to - Thermometer 49C, as prescribed in ji able timer measuring to 0.2 s. co vering the range from 5 to 1000 g. i oils, calibrated in absolute viscosity i i the viscosity range of the coatings to r - .Is should differ in viscosity by at least 5 r : range of the Stormer is covered by oils having 0 iCU), 10 P (85 KU), and 14 P (95 KU). ds are silicone, hydrocarbon, lin.ucone and hydrocarbon oils cali.o.-tmercially available.4 Uncalibrated . - ;.y be calibrated with any apparatus . .is of absolute viscosity.5 load to produce 200 r/min to each :c sity value in poises to load in grams ..- mon:6 - T 10-rj + 906.6 p)/30 - io poises and r and weight carrier from the e string is wound evenly on the p itsecl biai: xd from Arthur H. Thomas Co., Vine uuolph, 9A 19105; Fisher Scientific Co., 711 ' or Byn-Gardner, Inc., Gardner Laboratory, fD 20910. j available from the Cannon Instrument Co., P. . Silicon-, oils are available from the Brookfield .. : - -' Cushinp St., Stoughton, MA 02072. suppliers. ;c:r. H., "Calculation of Viscosity From Stormer id Engineering Chemistry, Vol 34, 1942, p. 163. /son. W. H., "A Method for the Standardization of lomcxersT ASTM Bulletin. No. 16 L 1949. DUP050297240 D 562 3 I FIG. 1 Stormer Viscometer with Paddle-Type Rotor and Stroboscopic Timer Ar ; 8.2 Attach a 5-g weight onto the string and then release the brake. If the viscometer starts to run from this dead start and continues to run through several revolutions of the string drum, it is satisfactory for use. If it does not start unaided N' --1 in. = FIG. 2 F when the 5-g weight is applied, the instrument should be reconditioned. temperature of 9.2.1 If ties : 8.3 Check the dimensions of the paddle-type rotor. They record the teer should be within 0.004 in. (0.1 mm) of the dimensions end of test t > C shown in Fig. 2. 9.3 Wher d ' 8.4 Select two standard oils having assigned values of load equilibrium, r to produce 200 r/min within the range of the values expected ping air, a-' 5 for the coatings to be measured (see 7.1). platform of 8.5 Adjust the temperature of the standard oils to 25 immersed i 0.2"C. The temperature of the Stormer apparatus should be rotor. the same. If the specified temperature cannot be obtained, 9.4 Place , record the temperature of the oil at the beginning and end of determine test to 0.2'C. range of 2 8.6 Determine the load in grams to produce 200 r/min 9.5 Usim t; with each of the two oils, using either Procedure A described that will r v in Section 9 or Procedure B described in Section 10. revolution v 8.6.1 If the oil temperature was not at 25 0.2C during measurer the test, correct the measured load in grams for the deviation to make a from that temperature. 100 revou No t e 2--Load corrections for deviations of oil temperature from the specified temperature can be made by means of a previously established 9.6 Rereadings for plot ofload versus oil temperature (see Appendix XI). 8.7 If the measured load (corrected for any temperature deviation from standard) is within 15 % of the assigned load values for the oils, the Stormer apparatus can be considered to be in satisfactory calibration. 9, Procedure A (Without Stroboscopic Attachment) 9.1 Thoroughly mix the sample and strain it into a 1-pt ' (500-mL) container to within % in. (20 mm) of the top. 9.2 Bring the temperature of the specimen to 25 0.2C and maintain it at that temperature during the test. The 10. Proem 10.1 Fo of the spe 10.2 C ment to e 10.3 r: determine range free 10.4 U: (to the no if g s Graduation 1 Line iS 2 U.5. Gage) vo o nee of 0.004" With Stormer Viscometer :us should be the same, ire cannot be obtained, men at the beginning and he sc i'nen has reached tg a * > to avoid entraper i tediately on the , the , udle-type rotor is nark on the shaft of the or of the viscometer and ce 100 revolutions in the d in 9.4, select two loads idiru: (time to give 100 27 in .'3 s. Make these t, tin-, nt permit the rotor men ung the timing for / in 9.5 until two . tee within 0.5 s. mm- ,,) o 9.2) for the preparation :f tue tti oboscopic attachget fie viscometer and ' niutions in the r d ' --j, select a weight ice : i )0-r/min pattern DUP050297241 i; # D 562 CO . <Q O <A c S c Q> 1o cr co w 43 *2 (0 r w k. DU P050297242 D 562 (fig. 3) on the stroboscopic timer, that is, where the lines appear to be stationary. 10.4.1 Lines moving in the direction of paddle rotation indicate a speed greater than 200 r/min and therefore, weight should be removed from the hanger. Conversely, lines moving opposite to direction of paddle rotation indicate a speed less than 200 r/min and weight should be added. No t e 3--There are other patterns that appear at speeds other than 200 r/min (See Fig. 4). The pattern for 200 r/min should be determined before running any tests. 10.5 Repeat the determination in 10.4 until a consistent value of load is obtained (that is, to within 5 g). 11. Calculation 11.1 Procedure A: 11.1.1 Calculate the load to within 5 g, to produce 100 revolutions in 30 s by interpolating between the load weights recorded for the readings made between 27 and 33 s for 100 revolutions. 11.1.2 Correct the load determined for any deviation of the specimen temperature from the specified temperature (see Appendix XI). 11.1.3 If desired, determine from Table 1 the KU corre sponding to the load to produce 100 revolutions in 30 s. No t e 4--Table 1 has been constructed so that it is not necessary to interpolate between toads to obtain the KU corresponding to the load to produce 100 revolutions in 30 s. The table provides KU values computed for a range of 27 to 33 s for 100 revolutions. 11.2 Procedure B: 11.2.1 If desired, determine from Table 2 the KU value corresponding to the load to produce 200 r/min. FIG. 3 Stroboscopic Lines Opening When Tinier is Adjusted to Exactly 200 r/min FIG. 12. R 12.1 12.1.' revolt 12. 12. and' 25*C 12 13. I 13.; made reduc. ' each ( ' of vat : KU,; fount 13. ' shour 95 v mr con:. grax: 13. four ope: SUSP 12 % 14. F 14.1 vise. 60 t -Bring as Multiples that May be p-r/nr-in Reached Grams KU jrmation: produce 200 r/min (100 f ' he specimen during the test ; r'. u eti for any deviation from | ! ; cc ;dnre B was used. n which determinations were ive.. ,-if,ducible, two water- eac t of six laboratories on withm-laboratory coefficient % m load grams or 1.5 % in cc _nt of variation was i o. .a KU. dents, the following criteria acceptability of results at the i j 70 53 75 54 80 55 85 57 90 58 95 60 r : named on the same | : times should be - i fom 9 % in load o r-so imu 3- . each the mean of \ obtained by n be considered . in load grams or v .3 Slormer viscometer, XI.1 specimer ments s tempera load or results. XI.2 consider, consister XI.3 ; I I i : ; t| DUP0502 97243 1 1 II be 100 test rom i. vere ter- on ient 7o in was tena :the ame i be load n of i by ered ts or ter; Grams KU 70 53 75 54 80 55 85 57 90 58 95 60 Grams KU 100 61 105 62 110 63 115 64 120 65 125 67 130 68 135 69 140 70 145 71 150 72 155 73 160 74 165 75 170 76 175 77 180 78 185 79 190 SO 195 81 TABLE 2 Krebs Units Corresponding to Lc (For use with Stormer Viscometer Grams KU Grams KU Grams KU Grarn;-.; KU 200 82 205 83 300 95 400 104 500 112 210 83 215 84 310 96 410 105 510 112 220 85 225 86 320 97 420 106 520 112 230 06 235 87 330 98 430 106 530 114 240 as 245 88 340 99 440 107 540 Ilf 250 89 255 90 350 10Q 450 108 550 I K 260 30 265 91 360 101 460 109 560 11 270 91 275 92 280 93 285 93 290 94 295 94 370 102 380 102 390 103 470 110 480 110 490 111 570 11" 580 Hf? 590 lif 37 -V APPE 7 (Nonmandator I XI. EFFECT OF SPECIMEN TEMPER. Tl XI. I For maximum accuracy in determining the effect of specimen temperature on Stormer consistency, measure ments should be performed at three different specimen temperatures covering the range of interest. The change in load or KU per 1C change can be determined from these results. XI .2 It has been observed that the consistency of an oil is considerably more sensitive to temperature than is the consistency of a paint. XI.3 Some typical effects of temperatures on the consis- t< - ; ' ;5, 77ia American Society for Testing and Materials takes no position res with any item mentioned in this standard. Users of this standard am ax patent rights, and the risk of infringement of such rights, are entu This standard is subject ?o revision at any time by the responsible r // not revised, either reapproved or withdrawn. Your comments are in and should be addressed to ASTM Headquarters. Your comments ' :i technical committee, which you may attend. If you feei that your cmviews known to the ASTM Commtttee on Standards, 1916 Race St.. ` i ... SCO -;31 :V : \32 322 " 32 3; } 340 i:';n 350 1.V 360 134 3'f :ss v ) . : Grams KU 900 136 910 136 920 137 930 137 940 136 950 136 960 138 970 139 980 139 990 140 Grams KU 1000 140 1010 140 1020 140 1030 140 1040 140 1050 141 1060 141 1070 141 1080 141 1090 141 IENCY below: Value at re KU 8 value ;49 72 417 85 -.86 93 i 95 81 440 108 >00 95 425 105 Change per 1"C Change Load, KU g value 14 2.5 18 2.0 11 1.5 8 1.0 40 2.0 4 0.5 4 0.5 -ic asixxiadin connection the Aiirjry of any such years and standards ssponsible make your 6 DUP050297244 I Designation: D 609 - 90 Standard Practice for Preparation of Cold-Rolled Steel Pm. Varnish, Conversion Coatings, an* This standard is issued under the fixed designation D 609; the number h original adoption or, in the case of revision, the year of last revision. A ii. " superscript epsilon () indicates an editorial change since the last revision < 1. Scope 1.1 This practice covers various types of cold rolled steel panels and die procedures to be followed in their preparation for testing paint, varnish, lacquer, conversion coatings, and related products. 1.2 The procedures are as follows: Procedure A--Conversion coatings (phosphates, chromates, etc.) Procedure B--Vapor degreasing Procedure C--Solvent brushing Procedure D--Solvent wiping Procedure E--Alkaline cleaning 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Docoments 2.1 ASTM Standards: A 109 Specification for Steel, Carbon, Cold-Rolled Strip2 A 366/A 366M Specification for Steel, Carbon, Cold- Rolled Sheet, Commercial Quality2 D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Drycleaning Solvents)3 3. Summary of Practice 3.1 Several procedures for preparation and cleaning of steel test panels are described as shown in Table 1. 4. Significance and Use - 4.1 The procedures described in this practice are designed to provide steel panels with a uniform and reproducible surface for testing of paint, varnish, lacquer, conversion coatings, and related products. 5. Test Panels 5.1 Prepare the test panels from rust and stain-free cold-rolled steel as described in 5.2, 5.3, 5.4, and Table 1. The panels shall be made to a size and thickness as agreed upon between the purchaser and seller. Edges shall be smoc" CO-: for p: terx Oi-V'Si': ' - ' Cl';:V or vs pry u Cf at b mv . and d t> : a! it a p V: c . cr.:r r.,.; L ( '. ; C; ( :.- 1 This practice is under the jurisdiction of ASTM Committee D-i on Paint and Related Coatings and Materials and is the direct-responsibility of Subcommittee 001.27 on Accelerated Testing. Current edition approved Aug. 24, 1990. Published November 1990. Originally published as D 609- 41. Last previous edition D 609 - 73 (1980) 1 Annual Book ofASTM Standards., Vol 01.03. 3 Annual Book ofASTM Standards, Vols 05.01 and U6.03, 62 : - !;r r 3' -) if. m-. 'ht year of 3 o: ; -.v-oprcval. A : h. steel may have been ( h s i preventive compound - irage. However, long- X , irface may cause an n : once such stains inhibit ci'. panels shall be free of i / r, variation caused by ` i i niproduced by steel mil] *:z . .,:u; iinish is typical of mc-'i palaces on automobiles, x pa;ai.a)iy characterized aT alley distance and the 1 a. i ov.xver, conversion coating :h - arcs may vary because of d.-rcs. and surface condi- * : xi (or "ground") ax nil!. Flat polishing v'x -ue surface with : as and provide a ; r. ior testing. Flat- of the surface oa polishing signifi- : ; : performance of a a o .p ure of the steel irface contami ay removed as aay - ay, a minimum of removed. Care must be a.aaratus and after pa removal of grit a : i i c i vi a C ":ash produced by l .. rai. This smooth cities such as a it is desirable to abness. onel should be i immersing 4 rod water. The film over the Pets or other ! : ! aversion coatliable from a *: or process >. Follow tbs mar sion mot app witf coat afte 6. in a tricl solv satii wit! be rem N prod ther 6. the all : flus. XJP050297245 been round longse an nhibit xee of ed by Jl mill cal of whiles, erized id the oating use of rondi- 'Und") ishing with vide a Flatce on lignifilce of steel itamived as am of ist be after >f grit ed by nooth uch as ible to 0 N' -- Pin- * microinches: nm = nanometer. Type No. Description 1 "2 3 Cold-rolled steel, as roiled (matte) Cold-rolted steel, fiat-polished one side Cold-rolled steel, as rolled (smooth) TABLE 1 Thickness, in. (mm) 0.02 to 0.038 (0.6 to 1.0) 0.024 to 0.038 (0.6 to 1.0) 0.010 to 0.024 (0.25 to 0.6) manufacturer's directions as to the application of the conver sion coating. Preparation of test panels may consist of one or ore steps of cleaning, rinsing, or conditioning prior to the application of the conversion coating. Additional rinsing uath water will usually be required after the conversion coating is applied. To prevent rust, force dry immediately after rinsing. 6.3 Procedure B: Vapor Degreasing--Suspend the panels in a vapor-phase type degreaser containing stabilized 1,1,1ttichloroethane and allow them to remain above the boiling solvent. When the panels attain vapor temperature, conden sation of vapor onto the panels no longer occurs. Prewiping with a clean lintless cloth saturated with mineral spirits may be necessary, since vapor degreasing generally does not remove solid particulate matter such as dirt, etc. (see Note). N' --Other organic solvents or combinations of solvents that will produce a water-break free surface may be used if agreed upon between the purchaser and the supplier. 6.4 Procedure C: Solvent Brushing--Power-brush scrub the panel with mineral spirits (Specification D 235). When all soluble and loosely adhering soil has been washed off, flush with clean mineral spirits. Dry at a temperature of 125 The American Society for Testing anil Materials takes nopositior. ;a with any item mentioned in this standard. Users of this standard s patent tights, and the risk of Intringement of such rights, are entire'./ This standard is subject to revision at any time by the responsibl e; ifnot revised, either reapproved or withdrawn. Your comments are i.i j and should be addressed to ASTM Headquarters. Your comments / technical committee, which you may attend. If you feel that your :. r,,views known to the ASTM Committee on Standards, 1916 Race Sr,. uld be sing a r. The /er the - other n coatfrom a ocesses ow the i 1 3t o i a t r ! M Specification A 109, A 366 A 109, A 366 A 109, A 366 e (see Note). ing clean lintless Ay rub the panel ing soil has been temperature of ye (see Note), aeous alkaline .ces as propriyanels with an or immersion, emendations of y of rinsing with of cleaning. To ymiug. not to be used ; orcgnated with vitent volatile rnroof bag or rnts, do not y . Handle the gloves. '; :`C ' i`f UP050297246 Designation: D 610 - 85 (Reapproved 1989)61 Standard Test Method for Evaluating Degree of Rusting on Ps? f This standard is issued under the fined designation D 6 LO; the number im original adoption or, in the case of revision, the year oflast revision. A num!; superscript epsilon () indicates an editorial change since the last revision or ,, This method has been approvedfor use by agencies of the Department of Dejii-. StandardNo. 141A. Consult the DoD Index ofSpecifications and Standardsforii.i Department ofDefense. ** Nora--Editorial changes were made throughout, including the title, in Oc; :b - 1. Scope 1.1 This test method covers the evaluation of the degree of rusting on painted steel surfaces using visual standards. These visual standards2 were developed in cooperation with the Steel Structures Painting Council (SSPC) to further standardization of methods. 1.2 This standard may invoke hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 Adjunct: D610 Degree of rust (four photos)2 3. Significance and Use 3.1 The amount of rusting beneath or through a paint film is a significant factor in determining whether a coating system should be repaired or replaced. This test method provides a standardized means for quantifying the amount of rust present 4. Interferences 4.1 The colored photographic reference standards and the associated rust-grade scale cover only rusting not accompa nied by blistering and evidenced by visible rust 4.1.1 Rust blistering beneath paint may be graded using the same scale by assuming the rust was completely visible and noting that the rusting was rust blistering. 1 This tea method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.46 on Industrial Protective Painting. This tea method has been jointly approved by ASTM and the Steel Structures Painting Council. Current edition approved Oct. 25, 1985. Published December i 985. Originally published as D 610 -41. Last previous edition D 610-68 (1981). ! The colored photographic reference standards are available at a nominal cost from ASTM Headquarters (requea Adjunct No. 12-406100-00), and from the Steel Structures Painting Council, 4400 5th Ave., Pittsburgh, PA 15213. 4.2 requi; 4.2 not 4.2.. accir 4. ' iron not 4.2. area i: single struct 4.2.' to the app; as u such 5. Pr-re 5. refer ruste desc T Nor : functi the g ofru; to rut . lusted ; to 10 Nr exan 5. for t the j area 52 terir were Jc Paint 64 'nc Council SPC*Vis*2 i -;t idards2 : : :1g must ry make .It. Iron or ; should r a given cling a -c area or I be given be more rust, such " color, graphic rhe area verbal etonential g have us area rade 10 i ie area i: rheO 1 show ;uired . ;.i upon ressing .ie Wis es as ifit ' !J P050297247 ouncit -Vls-2 rds2 aust take i or nild ven ig a 1 or ven lore uch >Ior, )bic irea rbal tial ave rea 10 tea eO iOW Lred pon sing ilisifit tines 0.0# o.: 6 * 9 * r. * . 1* Jr 3 wr . . *. 2 r-v Vf: . r* L M * # ; , " l&jo 33 RG. 1 Examples t> DUP050297248 # D 610 TABLE 1 Scale and Description - Rust Grades'* Description 10 no rusting or less than 0.01 % of surface rus ; 9 minute rusting, less than 0.03 % of surface n . 8s few isolated rust spots, less than 0.1 * of su 7 less than 0.3 % of surface rusted 6 extensive rust spots but less than 1 % of su; 5 rusting to the extent of 3 % of surface raster; 4 rusting to the extent of ID % of surface rust?: 3* approximately one sixth of the surface ruste 2 approximately one third of the surface raster; 1 approximately one half of the surface rusted 0 approximately 100 % of surface rusted A Correspond to Swedish Pictorial Standards for Rusting (1955) (black and white). B Corresponds to SSPC Initial Surface Conditions E and British Iron and Steel Research A( . e Corresponds to SSPC Initial Surface Conditions F and BISRA1.0 %. Corresponds to SSPC Initiaf Surface Condition G. Rust grades below 4 are of no practical importance in grading performances of paints. F Corresponds to SSPC Initial Surface ConcStion H. The American Society for Tasting and Materials takas no position respectin' with any item mentioned in this standard. Users of this standard are express patent rights, and rite risk of infringement of such rights, are entirely their oiv This standard is subject to revision at any time by the responsible technic ifnotrevised, either reapproved or withdrawn. Your comments areinvited eitt and should be addressed to ASTM Headquarters. Your comments will race/ technical committee, which you may attend. If you feel.that your comments : views known to the ASTM Committee on Standards, 1916 Race St., Phifaden 66 U-Si 'hot St; :vd unrv Wo. Wo. nom NO. non- Mo. TirOor nor unn- .con far ve 'd rm I. Sc 1.1 resist blast< such; 1.2 probh user . health limita 2. Re 2.1 D8. T T D9( C Dl< t: Dll D to D lo D Pi E1 P 3. Tet 3.1 3.1. to wea 4. Suit 4.1 / stream substrai unit fill the coa 1 This ? and Relau mitice EX) Currem published 2 Annuc 3 Anmu DUP050297249 Designation: D 658 - 91 Standard Test Method for Abrasion Resistance of Organs Abrasive1 This standard is issued under the fixed designation D 658; the nr, original adoption or, in the case of revision, the year of last revisio n superscript epsilon (e) indicates an editorial change since the Iasi : 1. Scope 1.1 This test method covers the determination of the resistance of organic coatings to abrasion produced by an air blast of abrasive on coatings appiied to a plane, rigid surface, such as a metal or glass panel. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D968 Test Method for Abrasion Resistance of Organic Coatings by Falling Abrasive2 D1005 Test Methods for Measurement of Dry Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 E 11 Specification for Wire-Cloth Sieves For Testing Purposes3 3. Terminology 3.1 Description of Term Specific to This Standard: 3.1.1 abrasion resistance--the weight of abrasive required to wear through a unit film thickness of the coating. 4. Summary of Test Method 4.1 An abrasive under the action of a controlled air stream is allowed to impinge on a coated panel until the substrate becomes visible. The amount of abrasive used per unit film thickness is reported as the abrasion resistance of the coating. ______________ ' This test method is under the jurisdiction ofASTM Committee D-l on Paint end Related Coatings and Materials and is the direct responsibility of Subcommittee D01.23 on Physical Properties of Applied Paint Films. Current edition approved Feb. 22, 1991. Published April 1991. Originally Published as D 658 - 42 T. Last previous edition D 658 - 61(1986)*'. 2 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards. Vol 14.02. SV ; Hi 67 : : year of : oprovaL A d) 068 are two Ostance of the same ;d useful in ' coatings. W digs. 1 and 2 Fig. 3. The >ntal. f the abrasive the throat of om ASTM 050297250 FIG. 2 Abrasion Test Apparatus (Open) the holder. Insect screen (approximately 270 openings per square inch) is suitable for this purpose. 6.2 Air Supply, oil-free, under pressure, capable of main taining a selected pressure within 200 Pa. 6.3 Standard Abrasive*--Silicon carbide grain passing a No. 170 (90-pm) sieve and retained on a No. 200 (75-p.m) sieve. No t e 2--To obtain maximum accuracy and precision of results, the abrasive should be sieved for a minimum of V2 h with vigorous agitation, and only that portion which passes through a No. 170 (90-)im) sieve and is retained on a No. 200 (75-p.m) sieve should be used in the test. The retained portion of the abrasive is considered satisfactory if a minimum of 85 % by weight meets the grain size requirements of 90 to 75 pm. Use the sieves described in Specification Ell. 7. Specimens 7.1 Apply uniform coatings of the material to be tested to a plane, rigid panel, such as metal or glass. Prepare a minimum of two coated panels for the material. 7.2 Cure the coated panels under conditions of humidity and temperature as agreed upon by the purchaser and seller. No t e 3--The coatings should be applied in accordance with Test Methods D 823, or as agreed upon between the purchaser and the seller. No t e 4--The thickness of the dry coatings should be measured in accordance with Test Methods D 1005, D 1400, or D 1186. No t e 5--For the apparatus shown in Figs. 1 and 2, the coated panels should not be larger than 5 by 4 by 'M in. (125 by 100 by 6.3 mm) thick. seller, and en' 5 Suitable silicon carbide grain is Carborundum grain # 180GG obtainable from the Carborundum Co., P. O. Box 423, Electro Minerals Div., Niagara Falls, NY 14302,or 180-mesh silicon carbide obtainable from City Chemical Corp., 132W. 22nd St,, New York, NY 10011. Other grades of abrasive may be used when mutually agreed upon between the purchaser and the seller. 68 t the inner oil-free air ill provide a the purbe 45 2 3 kPa (100 rable to use a n found to be tage of the procedure >y allowing he amount he air preste until the rchaser and at 23 2C in the same om. 10. Pro 10.1 quantit: apparat specime supply '< standar. 10.2 pinchcc coating point a mately the wet shut oi abrasiw N' V) weigi opening a contaii 10.3 the test 10.4 wearp; N' reused, 1 is return the coat: grain sh. 10.5 coated II. Ca 11.1 calcula followt where: W= T= 11.2 04"1.0. rox. 004"LD. aprox. I DUP050297251 le inner -free air provide he pur45+2 Pa (100 to use a und to be of the ocedure illowing amount tir pres-ntil the iser and 23 2*0 he same I.D. 'ID. 10. Procedure 10.1 Place one test panel on the specimen stage. Pour a quantity of abrasive into the abrasive holder (funnel) of the apparatus. Lower the nozzle to touch the surface of the test specimen and close the door of the tester. Turn on the air supply and adjust it to the pressure reading established in the standardization of the apparatus. 10.2 Release the stream of abrasive by removing the pinchcock attached to the tubing, and allow to flow until the coating is wom through to the base metal. Consider the end point as having been reached when a small spot approxi mately 2 mm in diameter is wom through in the center of the wear pattern. When this point is reached, immediately shut off the abrasive stream and determine the weight of abrasive used. N' 7--The amount of abrasive used can be determined either by (7) weighing the abrasive in the funnel before and after a run, or by (2) opening the bottom ofthe abrasion tester, collecting the abrasive used in a container, and weighing the abrasive. 10.3 Repeat 10.1 and 10.2 for two additional locations on the test specimen. 10.4 Measure the thickness ofthe coating adjacent to each wear pattern. N ' 8--The silicon carbide grain from previous tests may be reused, provided it is sieved through a No. 100 (150-|J.m) sieve before it is returned to the holder in order to eliminate all of the large particles of the coating that chipped off during the abrasion test. The silicon carbide grain shall be replaced after it has been used five times. 10.5 Repeat 10.1 to 10.4 on at least one additional panel coated with the material under test. 11. Calculation 11.1 For each abrasion determination on a coated panel, calculate the abrasion resistance. A, in grams per mil as follows: A = WjT where: W = weight of abrasive used, g (to one decimal place) and T = thickness of coating, mils (to one decimal place). 11.2 Calculate the mean of the abrasion resistance values The American Society for Testing end Materials takes no positin' with any item mentioned in this standard. Users of this standard s patent rights, and the risk of infringement of such rights, are entire This standard is subject to revision at any time by the resporc if not revised, either reapproved or withdrawn. Your comments are:' and should be addressed to ASTM Headquarters. Your comment:- technical committee, which you may attend. If you feel that your views known to the ASTM Committee on Standards, 1916 Race S' ted panel and the for each coated ing conditioning ;ed for each area h area tested, h area tested, eh coated panel, the range of the y test of this test ed four types of ance, the withinndtobe 7 % with aboratories coeffireedom. Based on hould be used for 95 % confidence ined by the same hey differ by more ach the mean of i by operators in ed suspect if they due. gs); air blast abra- arters. Request RR;D01- tectlon uy such ars and Jards unsible a your OUP050297252 Last ASTM Designation: D 659 - 86e1 Standard Method of Evaluating Degree of Chalking of Extern This method covers the evaluation of the degree of chalking on white an i procedure used to transfer to a test fabric the chalk which is then compare;' Formerly under the jurisdiction of ASTM Committee D-l on Paint and was discontinued in 1990 and replaced by ASTM Test Methods D 4214. f Films.1 ' Annual Book ofASTM Standards, Voi 06.01. 70 4 D. cs the ethod Paint 1. Scope 1.1 The test methc checking o rily intends 2. Referen 2.1 AS1 D661 T. Exteri< D1150 Result 3. Defrniti' 3.1 chec films by s through th sary in eva visible (as observed u 4. Signifies 4.1 Sine method is illustration failure. 5. Types t 5.1 Mat are: 5.1.1 In breaks de* pattern. 5.1.2 Li the breaks parallel lin- 5.1.3 SVt surface of 1 This test r and Related C mittee DO 1.27 Current edi* Published as D 2 Annual Bi OUP050297253 Designation: D 660 - 87 es the ethod Paint Standard Test Method for Evaluating Degree of Checking This standard is issued under the fixed designation D660; the nuir1 original adoption or, in the case of revision, the year of last revision. superscript epsilon (} indicates an editorial change since the last xv.vi This test method has been approvedfor use by agencies ofthe Depart. Standard No. J41A andfor listing in the Dob Index ofSpecificatu 1. Scope 1.1 The illustrated reference standards included in this test method are representative of degrees and types of checking of exterior paint films. These standards are prima rily intended for comparative evaluation. 2. Referenced Documents 2.1 ASTM Standards: D661 Test Method for Evaluating Degree of Cracking of Exterior Paints2 D1150 Single and Multi-Panel Forms for Recording Results of Exposure Tests of Paints2 3. Definition 3.1 checking--that phenomenon manifested in paint films by slight breaks in the film that do not penetrate through the last applied coating. Where precision is neces sary in evaluating a paint film, checking may be described as visible (as seen with the naked eye) or as microscopic (as observed under a magnification up to ten diameters). 4. Significance and Use 4.1 Since checking is not easily recognizable, this test method is intended to provide, through definition and illustrations, a means of evaluating the degree of this film failure. 5. Types of Checking 5.1 Many types of checking are recognized, ofwhich some are: 5.1.1 Irregular Pattern Type--Checking in which the breaks develop in the surface of the film in no definite pattern. 5.1.2 Line and Short Parallel Type--Checking in which the breaks in the surface of the film are generally arranged in parallel lines. 5.1.3 Switch Type--Checking in which the breaks in the surface of the film form short and long irregular Ikes 1 This test method is under the jurisdiction of ASTM Committee D-l on Painf aid Related Coatings and Materials and is the direct responsibility of Subcom Jttittee D01.27 on Accelerated Testing. Current edition approved Oct. 19, 1987. Published December 1987. Originally published as D 660 - 44 T. Last previous edition D 660-44(1981)". 1 Annual Book ofASTM Standards, Vol 06.01. -jfc 'hi -- of T.'V'.... A - / :.<cd - h the breaks in three-pronged ; ik - er and forming the or-::-. g :r <e breaks in the r :ii s' nd. metric patterns tin- n >h the breaks in >; ;i dal short breaks oga: ng ; fight angles. C'vd - : which breaks in c patterns. These J ' ` ' :t. no he breaks in the -fi cse oval shapes hown in Fig. 1 , may vary over fid be rated. It is veral locations, G several types of entities of dirt, re. If necessary, fi* brushing with a t to damage the checking under ita obtained, the dard D 1150 nr n.rchaser and the neen established a courtesy of TMO ^.'cstraat 9*?, P-'% OUP050297254 VJP0502 255 TOO 2 TOO 6 TOO 2 TOO '6 FIG. 1 'iUPOrSO? 256 257 Y i- A ASTM 8 TOO 2 A >c ^' v' r // >> ASTM 4 TOO 6 FIG. " 5 f i. i / / DU05 02 ,-258 259 < 2 TOO 6 FIG. 1 (' ifow in i -. Dlir->050/.;>7260 D !J P 0 5 0 2 9. 7261 TNO 2 Q C, 0 o w *o o .- k <% c c ASTM. 4 TNO 6 FIG. : r.; fj, S"; JP050297262 FIG. 2 No. S (Checking Magnified 10 Diameters) The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. J. Sc 1.1 crack stand "' jj ' j D1 I 2.2 Pic 3. Dt 3.1 by a i this i crack magn where check 4. Si 4.1 test n faiiur 5. T> 5.1 ' Th and Re mitiee ] Curr Publish. 2 An l 3 Co | publicai I Federat [ pA 194 Primary ; method 80 DUP050297263 Designation: D 661 - 86e1 Standard Test Method for Evaluating Degree of Cracking of Exterior Paints1 This standard is issued under the fixed designation D 661; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 647i ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. ei No t e--Footnote 3 was editorially changed in December 1988, I.Scope 1 i This test method covers the evaluation ofthe degree of -racking of exterior paints by comparison with photographic 5tandards. 2 Referenced Documents 2.1 ASTM Standards: p660 Test Method for Evaluating Degree of Checking of Exterior Paints2 DI150 Single- and Multi-Panel Forms for Recording Results of Exposure Tests of Paints2 2.2 Other Standards: Pictorial Standards of Coating Defects Handbook3 3. Definition 3.1 cracking--that phenomenon manifested in paint films by a break extending through to the surface painted. Where this is difficult to determine, the break should be called a crack only if the underlying surface is visible. The use of a magnification of 10 diameters is recommended in cases where it is difficult to differentiate between cracking and checking (see Test Method D 660). 4. Significance and Use 4.1 Cracking failure of paint films can occur in use. This test method provides a means of evaluating the degree ofthe failure by comparing the pictorial standards. 5. Types of Cracking 5.1 Three types of cracking are recognized: ' This test method is under the jurisdiction of ASTM Committee D-l on Paint "4 Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.27 on Accelerated Testing. Current edition approved Aug. 29, 1986. Published October 1986. Originally Published as D 661 - 42 T. Last previous edition D 661 - 44(1981)". '^Annual Book ofASTM Standards, Vol 06.01. Copies of the pictorial photographic reference standards are contained in the Publication Pictorial Standards ofCoatings Defects and may be obtained from the '(deration of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, ' 19422. The silver halide-gelatin photographs are intended to be the only ""naiy reference standards for this method. The reproductions ofthem in this test bmhod are for the purpose of illustration only. 5.1.1 Irregular Pattern Type--Cracking in which the breaks in the film are in no definite pattern. 5.1.2 Line Type--Cracking in which the breaks in the film are generally arranged in parallel lines, usually either horizontally or vertically, over the surface of the film. These breaks often follow the line of brush marks. 5.1.3 Sigmoid Type--Cracking in which the breaks in the film form a pattern consisting of curves meeting and intersecting, usually on a relatively large scale. 6. Use of Photographic Reference Standards 6.1 The photographic reference standards that are part of this test method and are provided in the Pictorial Standards ofCoating Defects Handbook are representative of the degree of cracking of exterior paint films. Figures 1 and 2 are for illustration purposes only and should not be used for evaluation. 6.2 The use of the photographic reference standards3 illustrated in Fig. 1 requires the following precautions: 6.2.1 The accompanying photographic reference stand ards show line-type cracking only. Irregular and sigmoid-type cracking may also be interpreted from these photographs. 6.2.2 Care must be taken not to confuse various types of failure that may be present on the same surface. This is particularly true in observing cracking and checking. Cracking may very often be an advanced stage of checking and is very often in evidence along with checking and other failures. 6.2.3 It must be realized that the degree of failure will vary over any given area. Therefore, an average portion of the film should be used for comparison. On larger surfaces it is recommended that ratings be made at several locations and the mean and range reported. 6.2.4 Paint films may collect excessive quantities of dirt, which may mask the type and degree of failure. If necessary, dirt should be removed by careful and gentle brushing with a moderately soft brush. 6.2.5 In examining wood panels for cracking failure, the ` possibility of wood failure should be recognized. This takes the form of a cracking or splitting of the wood itself with a resultant rupture of the paint film. Also, some panels will develop "resin spewing" which will cause early failure by cracking. These points should be taken into consideration in any evaluations. 6.3 For convenience in recording the data obtained, the 81 DUP050297264 ---------------------------------------- ---------------------------------------------------- ------- # D 661 V i No. 4 FIG. 1 Degrees of Cracking No. 2 records may be kept on forms such as Standard D 1150.4 7. Precision and Bias 7.1 No precision or bias statement has been established for this test method. "These record sheets may be obtained from ASTM Headquarters (order Adjunct No. 12-411500-11 and 12-411500-21) and from the Federation of Societies for Coatings Technology. 1315 Walnut St., Suite 832, Philadelphia, PA 19107. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and tha risk of iriringemerit of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. : I ero stai 2. ! r 41 | 1: 3. - by ; unt ; of s ; of ( ' 4. ti 4! tes! fai ! 5. Set an<3 mill C publ 3 publ Feck PA priir met! 82 DUP050297265 Designation: D 662 - 861 Standard Test Method for Evaluating Degree of Erosion of Exterior Paints41 1 This standard is issued under the fixed designation D 662; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision, A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 6431 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. 41 No t e--Footnote 4 was editorially changed in December 1988. 1. Scope 1.1 This test method covers the evaluation of the degree of erosion of exterior paints by comparison with photographic standards. 2. Referenced Documents 2.1 ASTM Standards: D659 Method of Evaluating Degree of Chalking of Exterior Paints2 D1150 Single- and Multi-Panel Forms for Recording Results of Exposure Tests of Paints2 2.2 Other Standards: Pictorial Standards ofCoating Defects Handbook3 3. Definition 3.1 erosion--that phenomenon manifested in paint films by the wearing away of the finish to expose the substrate or undercoat. The degree of failure is dependent on the amount of substrate or undercoat visible. Erosion occurs as the result of chalking. {See Method D 659 for evaluation of chalking.) 4. Significance and Use 4.1 Erosion failure of paint films can occur in use. This test method provides a mean of evaluating the degree of failure by comparing to pictorial standards. 5. Types of Erosion 5.1 Only one type of erosion is recognized, as defined in Section 3. 1 This test method is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.27 on Accelerated Testing. Current edition approved Aug. 29, 1986. Published October 1986. Originally published as D 662 -42 T. Last previous edition D662 - 44(1981)**. 1 Annual Book ofASTM Standards, VoL 06.01. 3 Copies of the pictorial photographic reference standards are contained in the publication Pictorial Standards ofCoatings Defects and may be obtained from the federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. The silver halide-gelatin photographs are intended to be the only Primary reference standards for this method. The reproductions ofthem in this test method are for the purpose of illustration only. 6. Use of Photographic Reference Standards 6.1 The photographic reference standards that are part of this test method and are provided in the Pictorial Standards ofCoatingJDefects Handbook are representative of the degree of erosion of exterior paint films. Figure 1 is for illustration purposes only and should not De used for evaluation. 6.2 The use of the photographic reference standards3 illustrated in Fig. 1 requires the following precautions: 6.2.1 Care must be taken not to confuse various types of failure that may be present on the same surface. 6.2.2 It must be realized that the degree of failure will vary over any given area. Therefore, an average portion of the film should be used for comparison. On larger surfaces it is recommended that ratings be made at several locations and the mean and range reported. 6.2.3 The photographic standards used represent various degrees of erosion of a white brushing type paint over a dark primer. This system was necessary to provide sufficient contrast for photographic purposes. The erosion of a film to its normal substrate is, however, readily visible to the naked eye so it may easily be compared to the standards and given a numerical rating. 6.2.4 In doubtful cases, erosion is sometimes more visible in a damp film than in a dry film. Also, with severe erosion, it is often easier to rate the degree of erosion in a damp film than in a dry film. 6.2.5 While erosion ofa sprayed film is more regular in its wearing away, a numerical rating can be given to it by interpreting the amount of erosion in terms of these stan dards. 6.3 For convenience in recording the data obtained, the records may be kept on forms such as Standard D 1150.4 7. Precision and Bias 7.1 No precision or bias statement has been established for this test method. "These record sheets may be obtained from ASTM Headquarters (order Adjunct No. 12-411500-11 and 12-411500-21) and from the Federation of Societies for Coatings Technology. 83 DUP050297266 ( D662 No. 8 No. 6 The American Society for Testing andMaterials takes no position respecting the validity ofanypatent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time try the responsible technical committee and must bs reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard ortor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a masting of the responsible technical committee, which you may attend, it you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 84 1. Scopt 1.1 TJ mining t wheel. 1.2 77 ations, a , address ethe respt j approprit ; applicabi ; 2. Refert 2.1 Ai D200C Ante 3. Signif 3.1 Th . used only results of 1 4. Appar | 4.1 Th | steel cylin with two i dimensioi 4.2 Th 1 cylinder j complete S). ` 4.3 Th : are showi ; 4.4 Th rubber or HK. 715 c 4.5 Tht i 1 This test and Related < ! mitteeDOL* : Current ei ; published as \ : 2 Annual b 3 An appai Co., Station 9 DU P050297267 Designation: D 71II - 89 Standard Test Method for No-Pick-Up Time of Traffic Paint1 This standard is issued under the Fixed designation D711; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. , Scot* 1 This test method covers a laboratory test for deter ging the no-pick-up time of a traffic paint by a rubber [ 2 This standard may involve hazardous materials, opero!!St and equipment. This standard does not purport to Egress all ofthe safety problems associated with its use. It is if responsibility of the user of this standard to establish iaropdote safety and health practices and determine the fiplicability of regulatory limitations prior to use. i Referenced Document 2.1 ASTM Standard: P200C Classification System for Rubber Products in Automotive Applications2 3, Significance and Use 3.1 This test method serves as a control test and should be used only as such. There is no direct correlation between the results of this test and field applications. 4. Apparatus 4.1 The apparatus3 as shown in Fig. 1 shall consist of a peel cylinder of the shape and dimensions as indicated, fitted with two replaceable O-rings and a ramp of shape and dimensions as shown. 4.2 The detailed dimensional requirements of the steel cylinder are given in Fig. 1. The total weight of the assembly complete with O-rings shall be 11 lb 14 oz 1 oz (5386 28 ) 4.3 The detailed dimensional requirements of the ramp are shown in Fig. 1. 4.4 The replaceable O-rings shall be made of synthetic rubber or rubber-like material meeting the requirements of HR 715 of Specification D 2000. 4.5 The dimensional requirements of the O-ring are as ' This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.44 on Traffic Paints. Current edition approved May 26, 1989. Published July 1989. Originally Published as D 711 - 43. Last previous edition D 711 - 84. 2 Annual Book ofASTM Standards, Vols 09.01 and 09.02. 5 An apparatus meeting the requirements is available from Paul N. Gardner Co.. Station 9, P.O. Box 6633, Fort Lauderdale, FL 33316. follows: Outside diameter Inside diameter Cross section 5. Procedure 4'A in. (104 mm) 3% in. (85 mm) % in. (9.5 mm) 5.1 Prepare a test stripe at least 3 in. (75 mm) in width of the paint to be tested by a mechanical spreader, or other suitable means on a clean plate glass panel at a wet film thickness of- 15 0.5 mils. (Use a plate glass panel approximately 4 by 8 by Vis in. (100 by 200 by 3 mm).) 5.1.1 Record the time of application. Allow the panel to dry in a horizontal position under the laboratory conditions specified (73.5 3,ST (23 2C) and 50 5 % relative humidity). 5.1.2 Test the paints used with drop-in beads without beads unless otherwise specified or agreed upon between the purchaser and the seller. 5.2 Butt the glass plate against the ramp. At regular intervals remove the wheel from its rest, hold against the rest as a starting point, then free roll the weighted wheel down the inclined ramp and over the paint film with each roll of the wheel over a new wheel path. Position the wheel properly so that a clean surface of the wheel will come into contact with the paint film. As many as three passes of the wheel can be made before the wheel needs to be cleaned. This can be done with a rag saturated with acetone. It is best to set aside the wheel after washing until all the solvent has evaporated. 5.3 Note the end point for no-pick-up time when no paint adheres to the rubber rings of the test wheel when it is rolled over the paint film. As the end point is approached, roll the weighted wheel over the paint film every 30 s. 6. Report 6.1 Report the time elapsed between application of the paint and the end point as the drying time for no-pick-up of the traffic paint. 7. Precision and Bias 7.1 Precision--Because of the poor precision of this test method, if it is used in a specification, the maximum deviation from the maximum no-pick-up time specified should be agreed upon between the purchaser and the seller. 7.2 Bias--Bias cannot be determined. 8. Keywords 8.1 auto no-track time; drying time; traffic paint 85 DUP05 0297268 # D 711 FIG. 1 Traffic Paint Drying Time Wheel and Ramp--Dual Model The American Society for Testing and Materials takas no position respecting the validity ofany patent rights asserted in sormeotion with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity Of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Yourcomments are invited either for revision of this standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful cons/tterat/on af a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to tfte ASTM Committee on Standards, 191B Race St., Philadelphia, PA 19103. 86 DUP050297269 Designation: D 713 - 90 Standard Practice for Conducting Road Service Tests on Fluid Traffic Marking Materials*1 This standard is issued under the fixed designation D 713; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (f) indicates an editorial change since the last revision or reapproval. NOTE--Paragraphs 9.4 and 9.5 were inadvertently deleted and were reinstated in February 1990. 1. Scope I j This practice covers the determination of the relative service life of fluid traffic marking materials such as paint, thermoplastic, epoxy, and polyester products under actual road conditions using transverse test lines. Materials under test are applied under prescribed conditions and periodic observations are made using prescribed performance criteria. 1,2 This practice may involve hazardous materials, opera tions and equipment. This practice does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this practice to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D711 Test Method for No-Pick-Up Time of Traffic Paint2 0913 Test Method for Evaluating Degree of Resistance to Wear of Traffic Paint2 3. Significance and Use 3.1 This practice is an accelerated evaluation of bead retention and wear characteristics of fluid traffic marking materials. It is used to determine the useful life of such markings in the field. The same procedures are applicable to evaluating longitudinal lines to determine service life. 4. Type and Location of Pavement for Tests 4.1 Select sections where traffic is moderate and freerolling with no grades, curves, intersections, or access points near enough to cause excessive braking or turning move ments, where wear is uniform with full exposure to the sun throughout daylight hours, and there is good drainage. Select surfaces that are representative of the pavements upon which the fluid traffic marking material will be used in practice. Such surfaces include portland cement concrete, sheet as phalt, bituminous concrete, rock asphalt, and bituminous surface treatment. 1 This practice is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee 001.44 on Traffic Coatings. Current edition approved February 15, 1990. Published April 1990. OriginaUy published as D 713 - 43 T. Last previous edition D 713 - 87. 1 Annual Book ofASTM Standards, Vo! 06.01. 5. Conditions at Time of Application 5.1 Clean the test area thoroughly of all foreign material. Do not apply traffic paint when the pavement surface is damp or wet nor when the pavement temperature is below 50F (KFC). Application between 10 a.m. and 3 p.m. is recommended. During application record air and pavement temperature hourly. 6. Measurement of Wet Film Thickness 6.1 To aid in obtaining the correct film thickness, a length of roofing paper placed by the side of the road can be used. Place a rigid metal test panel on the roofing paper and in the path of the test line. A 12 by 12-in. (300 by 300-mm) metal panel Vie in. (1.5 mm) in thickness is satisfactory. Immedi ately after the test line is applied by the motorized striper, read the wet film thickness. If the wet film thickness is not satisfactory, adjust the spray pressure and repeat until the target wet film thickness is attained. It is important that no glass beads or other interfering materials be present that would give a false wet film reading. When the wet film thickness is correct, apply a test line across a tared metal panel and weigh immediately. A balance must be immedi ately available and be thoroughly shielded from wind as well as be of 1500-g capacity with 0.1 g or better sensitivity. As a basis for determination of glass bead application (7.1) the weight of a paint line 4 by 12 in. (without consideration for solvent loss) can be calculated as follows: W = 0.0943 X(XS where: W = weight of paint line, g, t = mil thickness, and g = weight per gallon, lb. 7. Measurement of Glass Beads 7.1 After the completion of 6.1, apply another test line to a tared panel with the motorized striper, this time also adding the glass beads, and weigh immediately. The weight difference between this measurement and that in 6.1 gives the amount of glass beads on the panel. The process can be repeated if an adjustment in the bead application rate is needed. The weight of applied glass beads can be calculated as follows: W -- 1.418 x B where: W -- weight of glass beads, g, and B = glass beads per gallon of paint, lb. 87 DUPO 502 97270 713 8. Application Procedure 8.1 Apply the test stripes 4 in. (100 mm) in width and transversely on the road. At the option of the purchaser, the test stripes may be applied to the pavement at an angle of 45 to the direction of the traffic, or longitudinally in each wheel path, in order to increase the area of contact with traffic. 8.2 Apply test stripes (trained personnel under the super vision of the purchaser) by using a pavement-marking machine similar to the production pavement marking equip ment. Apply the test stripes to at least two sections of each road surface selected to ensure against undetected road surface problems. When more than one specimen is tested at more than one location, change the sequence of placement to minimize the effect of time of day and time period before the test deck is opened to traffic. 8.3 Apply at least two lines of each specimen in each section for better statistical reliability. A tared panel as used in the measurement of glass beads (see 7.1) should be placed between the wheel track ofone line's application as a double check for material and glass bead application rates. Weights between this reading and that found in 7.1 should agree within 0.5 g. The purchaser may wish to place another smaller panel between the wheel tracks to retain for future reference. 8.4 The road surface test lines have a wet film thickness within 0.5 mil of that required by the purchaser. No t e 1--If no wet film thickness is specified, 15.0 mil is recom mended. 8.5 A fluid marking material with which the purchaser has had considerable production experience is included in the test series as a control. 8.6 Glass beads are placed in the paint film within 0.5 lb/gal of that required by the purchaser. All glass beads are supplied by the purchaser. No t e 2--If no bead application rate is specified, 6.0 lb/gal of paint is recommended. 9. Performance Criteria 9.1 Auto-No-Track Time--The auto no-track time is determined by passing over the freshly applied line in a simulated passing maneuver with a standard size passenger car with regular treads (no snow treads). A line showing no visual pick-up and redeposition of the materials onto the pavement surface when viewed from a distance of 50 ft in the highway direction is considered as showing no pick-up and conforming to the drying time requirements. 9.1.1 The test line is applied at the same temperature, the same wet film thickness, and the same rate of glass beads as will be specified by the purchaser in production application. 9.1.2 The no-track maximum time is measured when the pavement temperature is from 60 to 120F (15 to 50C) and under local humidity conditions, providing that the pave ment is dry. No t e 3--A laboratory no-track test is described in Test Method D711. This test is a laboratory control test and has little or no correlation with field results. Some paints have a tendency to skin over rapidly allowing the specimen to meet the maximum specified time for the laboratory test, but would be unsatisfactory at that time on a road surface. 9.2 Appearance--The impression of the observer of the general condition of the test lines when viewed without any detailed inspection, from a distance of at least 10 ft. It is a measure of satisfactory or unsatisfactory appeal to the observer. It includes a comparison of the color of the surface under consideration with the original color, taking into account changes due to yellowing, bleeding, darkening, fading, dirt collection, mold growth, etc. This determination is made in each wheel track in an area extending 9 in. (229 mm) each side of the point of greatest wear. The appearance is rated either acceptable or unacceptable. 9.3 Durability--The durability is equal to one tenth of the percentages of material remaining on the pavement (when examined by the unaided eye). This determination is made in each wheel track in an area extending 9 in. (229 mm) each side of the point of greatest wear. The percent of paint remaining on the pavement is considered as the percent of the prescribed area of test stripe in which the substrate is not exposed. Make the evaluations in accordance with Test Method D 913. * j ! l N' 4--In the absence of a specification by the purchaser, failure shall be a rating less than 4 (less than 40 % material remaining on the pavement). 9.4 Night Visibility--Night visibility designates the ap. parent brightness when examined at night under tungsten illumination from the side of the road, with eye and light source separated by 1% in. (40 mm) that corresponds to an observation angle of approximately Vi". Night visibility determinations are made in the wheel track areas used for rating durability, and are based on a factor of 10 for a unexposed standard panel placed next to the test stripe and 0 for no apparent brightness. N' 5--In the absence of a specification by the purchaser, failure shall be a rating less than 4. No t e 6--A new test method for night visibility using a retro- reflectometer is being developed which is expected to have much greater precision. J 9.5 Length of Useful Life--The length of useful life is determined by the number of days of duration between the date the sample was applied to the road surface and the date any one of the designated measurements falls below the specified minimum rating. 10. Evaluation Procedure 10.1 Make periodic inspections of the test sections in accordance with 9.2, 9.3, and 9.4. Record at each inspection the general daytime appearance (including color), film con dition, and night visibility (retro-reflectance). 10.2 Inspect the test lines at regular monthly intervals. As the test lines approach failure, they should be evaluated every 2 weeks (weather permitting). The test lines must be evalu ated until failure. Different types of traffic paint and mark ings do not wear out in a linear manner. Hence, it is not possible to extrapolate to failure some intermediate data. The winter season is also a must when evaluating test lines. 11. Calculation 11.1 Make cost calculations as follows: C = MjL x F where: C = cost per foot per day of useful life. A/= c* l = !f F = fe N' calculate perform; other flu ctiaractei available When le 88 DUP050297271 ut any It is a o the surface 8 into :eningi nation ' (229 stance ofthe (when made }) each ' Paint :ent of ' is not 11 Test ; failure 3 on the he apmgsten d light s to an isibility sed for for an aandO t, failure a retroli greater life is een the he date yw the D 713 jjss cost of paint per gallon, ^ * length of useful life in days as previously observed, and p = feet per gallon actually applied. MOTE 7--The cost of the glass beads is usually not included in the calculation because it will be a constant when comparing the relative performance of a specified class of paint Various types of paints and jlher fluid marking materials, however, can have different bead wetting characteristics, and beads with different wetting characteristics also are availably either of which could influence the useful life of the line, y/hen testing more than one type of material or one type of bead, the optimum cost/performance may be at a different bead application rate than that recommended in 8.6. 11.2 To determine the relative performance of the dif ferent fluid traffic marking materials during the course ofthe test, the following weighted rating, R, can be used: R = 030A + 0.30D + 0.40N where: A = appearance as defined in 9.2 and determined using a rating from 0 to 10, D = durability as defined in 9.3, and JV = night visibility as defined in 9.4. The American Society for Testing and Materials takes no position respecting the validity olany patent rights asserted in connection with any Item mentioned in this standard. Users ol this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard ss subject to revision at any time by the responsible technical committee and must be reviewed every five years and it notrevised, either reapproved or withdrawn. Your comments are invitedeither tor revision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 pane St., Philadelphia, PA 19103. ons in section m con- vals. As :d every 2 evalui markt is not te data, st lines. 89 DUP050297272 Designation: D 714 - 87 Standard Test Method for Evaluating Degree of Blistering of Paints1 This standard is issued under the fixed designation D 714; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 6461 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. 1. Scope 1.1 This test method employs photographic reference standards to evaluate the degree of blistering that may develop when paint systems are subjected to conditions which will cause blistering. While primarily intended for use on metal and other nonporous surfaces, this test method may be used to evaluate blisters on porous surfaces, such as wood, if the size of blisters falls within the scope of these reference standards. When the reference standards are used as a specification of performance, the permissible degree of blistering of the paint system shall be agreed upon by the purchaser and the seller. 2. Significance and Use 2.1 A phenomenon peculiar to painted surfaces is the formation of blisters relative to some system weakness. This test method provides a standard procedure of describing the size and density of the blisters so that comparisons of severity can be made. 3. Reference Standards 3.1 The photographic reference standards are glossy prints.2 Figures 1 to 4 are reproductions of these standards and are included to illustrate two characteristics of blistering: size and frequency. 3.2 Size--Reference standards have been selected for four steps as to size on a numerical scale from 10 to 0, in which 1 This test method is under thejurisdiction of ASTM Committee D-I on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.27 on Accelerated Testing. Current edition approved May 29, 1987, Published July 1987. Originally published as D 714 - 43 T. Last previous edition D 714 - 56 (1981). 2 Glossy prints of the photographic reference standards showing types of blistering are available at a nominal charge from ASTM Headquarters, 19 L6 Race St., Philadelphia, PA 19103. Request Adjunct No. 12-407140-00. No. 10 represents no blistering. Blistering standard No. 8 represents the smallest size blister easily seen by the unaided eye. Blistering standards Nos. 6, 4, and 2 represent progres sively larger sizes. 3.3 Frequency--Reference standards have been selected for four steps in frequency at each step in size, designated as follows: Dense, D, Medium dense, MD, Medium, M, and Few, F. No t e l--A quantitative physical description of blistering would include the following characteristics determined by actual count: Size distribution in terms of mensuration units, Frequency of occurrence per unit area, Pattern of distribution over the surface, and Shape of blister For the usual tests, an actual count is more elaborate than is necessary. 4. Procedure 4.1 Subject the paint film to the test conditions agreed upon by the purchaser and the seller. Then evaluate the paint film for the degree of blistering by comparison with the photographic reference standards in Figs. 1 to 4. 5. Reporting 5.1 Report blistering as a number (Note 2) designating the size of the blisters and a qualitative term or symbol indi cating the frequency. 5.2 Intermediate steps in size or frequency of blisters may be judged by interpolation. 5.3 When the distribution of blisters over the area has a nonuniform pattern, use an additional phrase to describe the distribution, such as "small clusters," or "large patches." No t e 2--The number refers to the largest size blister that is numerous enough to be representative of the specimen. For example, photographic standard No. 4, "Dense," has blisters ranging in size from about No. 7 to No. 4, inclusive. j ! : 5 1 , i !f 90 DUPO 502 97273 d No. 8 unaided progresselected nated as ng would nt: necessary. s agreed he paint vith the # D 714 4 *f f4 4 U4 4 4 I *4 Few Medium FIG. 1 Blister Size No. 2 4 1 DU P050297274 D 714 DUP050297275 D 714 | f l Few Medium FIG. 3 Blister Size No. 6 1 1 I I Medium Dense FIG. 3 Continued Dense i DUP050297276 D 714 Medium Few FIG. 4 Blister size No. 8 Medium Dense FIG. 4 Continued 94 DUP050297277 # D 714 The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and itnot revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration af a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 95 DU P05 029 7278 Designation: D 772 - 861 Standard Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints1 This standard is issued under the fixed designation D 772; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision, A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 6441 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. 1. Scope 1.1 This test method covers the evaluation of the degree of flaking (scaling) of exterior paints by comparison with photographic standards. 2. Referenced Documents 2.1 ASTM Standard: D1150 Single and Multi- Panel Forms for Recording Results of Exposure Tests of Paints2 2.2 Other Standards: Pictorial Standards of Coating Defects Handbook3 3. Definition 3.1 flaking (scaling)--that phenomenon manifested in paint films by the actual detachment of pieces of the film itself either from its substrate or from paint previously applied. Flaking (scaling) is generally preceded by cracking or checking or blistering, and is the result of loss of adhesion, usually due to stress-strain factors coming into play. 4. Significance and Use 4.1 Flaking (scaling) failure of paint films can occur in use. This test method provides a means of evaluating the degree of failure by comparing to pictorial standards. 5. Type of Flaking (Scaling) 5.1 Only one type of flaking (scaling) is recognized, as defined in Section 3. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.27 on Accelerated Testing. Current edition approved Aug. 29, 1986. Published October 1986. Originally published as D 772 - 44 T. Last previous edition D 772 - 47 (1981)ei. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Copies of the pictorial photographic reference standards are contained in the publication Pictorial Standards of Coatings Defects and may be obtained from the Federation of Societies for Coatings Technology, 492 Norristown Rd,, Blue Bell, PA 19422. The silver halide-gelatin photographs are intended to be the only primary reference standards for this method. The reproductions ofthem in this test method are for the purpose of illustration only. 6. Use of Photographic Reference Standards 6.1 The photographic reference standards that are part of this test method and are provided in the Pictorial Standards ofCoating Defects Handbook are representative of the degree of cracking of exterior paint films. Figure 1 is for illustration purposes only and should not he used for evaluation. 6.2 The use of the photographic reference standards2 illustrated in Fig. 1 requires the following precautions: 6.2.1 Care must be taken not to confuse various types of failure that may be present on the same surface. 6.2.2 It must be realized that degree of failure will vary over any given area. Therefore, an average portion of the film should be used for comparison. On larger surfaces it is recommended that ratings be made at several locations and the mean and range reported. 6.2.3 In technical literature, a distinction is sometimes made between flaking and scaling. In most cases, however, flaking and scaling refer to the same phenomenon. In some instances, the term flaking is used to describe the detachment of pieces of film less than 'A in. (6.4 mm) in size, and scaling, the detachment of pieces over lA in. in size. In other instances, the term flaking is used to describe the detachment of pieces of film from the immediate undercoat (intercoat failure) and scaling the detachment of pieces from the base (complete failure). It should be kept in mind that the flakes may vary widely in size and shape from those illustrated by the reference standards in Fig. 1, varying from a fraction of an inch to several inches in size. 6.2.4 Peeling is frequently due to a moisture condition and when this is evident it should be taken into consider ation in any evaluation. 6.2.5 For convenience in recording the data obtained, the records may be kept on forms such as Standard D f 150.4 7. Precision and Bias 7.1 No precision or bias statement has been established for this test method. 4 These record sheers may be obtained from ASTM Headquarters (order Adjunct No. 12-41150-11 and 12-41150-21) and from the Federation of Societies for Coatings Technology. 96 DUP050297279 art of dards iegree 'ation lards2 pes of 1 vary of the is it is is and etimes wever, i some hment scaling, other thment tercoat le base 5 flakes ated by ;tion of ndition insider- tied, the 150.4 ablished ters (order of Societies # D 772 No. 4 FIG. 1 Degrees of Flaking (Scaling) 97 DUPO 502 97280 T A A I D 772 f r r No. 8 FIG. 1 Degrees of Raking (Scaling) (Concluded) 98 DUP050297281 # D 772 TheAmerican Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of. such rights, are entirely their own responsibility. This standard is sub/ect to revision at any time by the responsible technical committee and musfbe reviewed every five years and Ifnotrevised, etherreapproved or withdrawn. Your comments are Invitedeither for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Commtttao on Standards, ISIS Race St., Philadelphia, PA 19103. -a ? . ; . j 99i DUP050297282 I Designation: D 822 - 89 Standard Practice for Conducting Tests on Paint and Related Coatings and Materials using Filtered Open-Flame Carbon-Arc Light and Water Exposure Apparatus1 This standard is issued under the fixed designation D 822; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovaL This standard has been approved for use by agencies cf the Department of Defense. Consult the DoD Index of Specifications and Standards for the specific year ofissue which, has been adopted by the Department cfDefense. 1. Scope 1.1 This practice covers accelerated exposure testing of paint, varnish, lacquer, and related products using filtered open-flame carbon-arc devices as described in Practice G 23. Two basic apparatus types are available for coating evalua tion since open-flame carbon-arc devices can be manufac tured with or without automatic humidity control. These are Types E and EH as described in Practice G 23.2 Each type of device can be operated with different types ofglass filters that filter various amounts of ultraviolet (UV) radiation. All references to use ofthis practice must include a description of the filter used. Table 1 describes commonly used test conditions. Interlaboratory comparisons must be made only with devices using the same filter type and test conditions. 1.2 Previous versions of this practice described exposures using either open-flame carbon arcs or enclosed carbon arcs. , N' 1--A new practice using enclosed carbon-arc exposure appa ratus is under development. Another procedure for exposing these products is covered by Practice D 33<i 1 in which the specimens are subjected to radiation from an unfiltered open-flame carbon arc that produces much higher levels of short wavelength radiation than filtered open flame or enclosed carbon arcs. Only automatic humidity con trolled open-flame carbon-arc apparatus (Type EH) is applicable to Practice D3361. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 4. 2. Referenced Documents 2.1 ASTM Standards: D358 Specification for Wood to Be Used as Panels in Weathering Tests of Coatings3 D 523 Test Method for Specular Gloss3 D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products3 1 This practice is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.27 on Accelerated Tests for Protective Coatings. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 822 - 45. Last previous edition D 822 - 86. 3 Apparatus and carbon arcs manufactured by Atlas Electric Devices Company, 4114 N. Ravenswood Ave., Chicago, IL 60613, have been found satisfactory for this purpose. 3 Annual Book ofASTM Standards, Vol 06.01. D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces3 D659 Method of Evaluating Degree of Chalking of Exterior Paints3 D660 Test Method for Evaluating Degree of Checking of Exterior Paints3 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints3 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints3 D714 Test Method for Evaluating Degree of Blistering of Paints3 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints3 D823 Test Methods for Producing Films of Uniform ' Thickness of Paint, Varnish, and Related Products on Test Panels3 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers3 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base3 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base3 D1729 Practice for Visual Evaluation of Color Differences of Opaque Materials4 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting5 D2244 Test Method for Calculation of Color Differences From Instrumentaliy Measured Color Coordinates3 D2616 Test Method for Evaluation of Visual Color Difference with a Gray Scale4 D3361 Practice for Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Flame Carbon-Arc Type) for Testing Paint, Varnish, Lacquer, and Related Prod ucts Using the Dew Cycle3 D 4214 Test Methods for Evaluating Degree of Chalking of' Exterior Paint Films3 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band! Filter Reflectometry6 G23 Practice for Operating Light-Exposure Apparatus | (Carbon-Arc Type) With and Without Water for Expo- 4 Annual Book ofASTM Standards, Vol 14.02. 5 Annual Bode ofASTM Standards, Vols 02.05 and 06.01. 6 Annua! Bode ofASTM Standards, Vols06.01 and 14.02. 100 Tt io; if if 1Q If 4E 12 3. DUP050297283 usting on liking of ecking of acking of rosion of stering of f Flaking Uniform >ducts on Dry-Film ;ters3 ement of 5 Applied ement of lings Ap- ifferences nd Alu- ferences tes3 1 Color Exposure .re Type) ted Prod- lalking of e Factor, oad-Band apparatus for Expo- 0 822 TABLE 1 Test Cycles Commonly Used for Carbon-Arc Exposure ' resting of Paints, Varnishes, Lacquers and Related Coatings Cycle Description Black Panel Temp/ op (oC) Typical Uses TjjjTmin light 18 min fight and water spray is h using: <02 min light tfl min light and water 9pray 5 h at 95 4 % relative humidity with no water spray 48 min light 12 min light and water spray 4 h light 4 h water spray 12 h light 12 h water spray 8 h light 10 h light and water spray 6 h water spray 145 5 general coatings (S3 2.5) 145 5 (63 2.5) 75 3 (24 1.5) general coatings 145 5 (63 2.5) 145 5 (63 2.5) 145 5 (63 2.5) 145 5 (63 2.5) original equipment manufactured coatings exterior pigmented paints exterior wood stains and clears marine enamels * Unless otherwise indicated, black panel temperature during light only portion of the cycle. s Historical convention has established this as a very commonly used test cycle. sure of Nonmetallic Materials4 3, Significance and Use 3.1 This practice is intended to evaluate coating films for their stability in apparatus that expose ultraviolet (UV) light and moisture. If die spectral power distribution of the light source used for exposure tests does not adequately simulate that of terrestrial solar radiation, it may produce a different type of degradation and distort the ranking of materials obtained in outdoor exposures. Figures 1 and 2 compare representative spectral power distributions of the open-flame carbon arc (with two different types of glass filters) with that ofterrestrial sunlight. Soda borosilicate glasses remove more short wavelength UV radiation than potash lithia glasses7 and their use can provide carbon-arc exposures that are a better approximation of terrestrial solar UV. Exposures using soda borosilicate glass filters will typically take longer to produce photochemical degradation. 3.2 No single operating procedure for light-exposure ap paratus with or without water can, be specified as a direct simulation of natural exposure. This practice does not ex press, or imply, a specific correlation with outdoor exposure. 3.3 Since natural environments vary with respect to climate, geography, and topography, it may be expected that the effects of natural exposures will vary accordingly. Fur thermore, all materials are not affected equally by the same environment. Therefore, results obtained by use of this practice should not be represented as equivalent to those of any natural weathering test until the degree ofcorrelation has been empirically established for the material in question. 3.4 Variations in results are possible between instruments of the same type operating within the accepted limits of this practice. It is recommended that results obtained using this practice be compared with those of a control or reference 7 Pyrex No. 7740 and Corex No. 7058 Glass Filters, manufactured by Corning Glass Works, Coming, NY 14831, or equivalent, have been found satisfactory for this purpose. Sunlight 3with 2.5mm Corex with nm Pyrex *7058 filter 17740 filter IRRADIANCE (wttt*/m2tonn) N' --Sunlight was measured In Phoenix, AZ, at the summer solstice with clear sky at solar noon using a double grating monochromator (1-nm bandpass) with a quartz cosine receptor on an equatorial follow-the-sun mount. The carbon arc irradiance was measured at the sample plane centered within the allowed sample area. Because of momentary fluctuations in Intensity due to flickering of the carbon arc flame, the spectral power distributions shown in this figure are representative and- are not meant to be used to calculate or estimate total radiant exposure for tests in carbon-arc devices. FIG. 1 Representative Spectral Power Distributions (250 to 400 nm) for Terrestrial Sunlight and Open Flame Carbon Arc Using Two Types of Glass Filters Sunlight with J.Snin Corex #7058 Fi!ter IRRADIANCE 6mttAn2/nnd with 3nn Pyrex #7740 filter N' --Measurements made as described in Fig. 1. Because of momentary fluctuations in Intensity due to flickering of the carbon arc flame, the spectral power distributions shown In this figure are representative and are not meant to be used to calculate or estimate total radiant exposure for tests in carbon-arc devices. FIG. 2 Representative Spectral Power Distributions (250 to 300 nm) for Terrestrial Sunlight and Open Flame Carbon Arc Using Two Types of Glass Filters material that is mutually agreed upon between the interested parties. 3.5 All references to exposures in accordance with this practice must include a complete description ofthefilterglass and test cycle used. 4. Hazards 4.1 Precaution--In addition to other precautions, never look directly at the carbon arc because UV radiation can damage the eye. Most carbon-arc machines are equipped 101 DU P05 02 972 84 D 822 with door safety switches, but users of old equipment must be certain to turn the OPERATE switch to OFF before opening the test-chamber door. 4.2 The burning carbon rods used in these devices become be agreed upon between all interested parties. 6.3 It is recommended that the temperature of the water used for specimen spray be 60 9? (16 5C). Water used for specimen spray must meet the purity levels specified in # very hot during use. Make sure to allow at least 15 min for Practice G 23 in order to avoid unrealistic water spotting. the arcs to cool after the device is turned off before 6.4 When mutually agreed upon, cycles other than those attempting to change the carbon rods. Avoid inhaling ash listed in Table 1 may be used. The term "cycle" is defined as dust when changing carbon rods. the set of exposure conditions (light, light plus water spray, dark periods) that are repeated. 5. Test Specimens 5.1 Apply the coating to flat (plane) panels with the 7. Periods of Exposure substrate, method of preparation, method of application, 7.1 Use one of the following methods to determine the coating system, film thickness, and method ofdrying consist duration of the exposure under this practice: ent with the anticipated end use, or as mutually agreed upon 7.1.1 A mutually agreed upon specified number of total between the producer and user. - 5.2 Panel specifications and methods of preparation in hours. 7.1.2 The number of total hours of exposure required to 1. Scope ri clude but are not limited to Methods D 609, Specification D 358, or Practice D 1730. Select panel sizes suitable for use with the exposure apparatus. 5.3 Coat test panels in accordance with Test Methods D 823 and measure the film thickness in accordance with an appropriate procedure selected from Test Methods D 1005, D 1186, or D 1400. Nondestructive methods are preferred because panels so measured need not be repaired. 5.4 Prior to exposing coated panels in the apparatus, produce a mutually agreed upon amount of change in either the test specimen or an agreed upon control or reference material. 8. Evaluation of Specimens After Exposure 8.1 Determine the changes in exposed test specimens in accordance with ASTM Test Methods D 523, D 610, D 659, D 660, D661, D 662, D714, D772, D2244, D2616, D4214, E97 and Practice D 1729. Consider product use 1.1 Fi' uniform methods ; Test Met Test Met Test Met I Test Met ! Test Met \ 1.2 Th condition them at 73 3F (23 2C) and 50 5 % relative humidity for one ofthe following periods in accordance with requirements when selecting appropriate methods. 8.2 Evaluate test specimens by ranking their performance safety pr, responsib the type of coating: relative to a control or reference material exposed at the same time. priate saj bility ofr. Baked coatings Radiation-cured coatings Ail other coatings - 24 h 24 h. 7 days 8.3 Plot properties of test specimens and controls as a function of exposure time and compare rate of change with 2, Refere N' 2--The procedures and specifications described in 5.2 through that of the control or reference material. When this method I 2.1 AS 5.4 are recommended but others may be used if agreed upon between all of evaluation is used, the control or reference material must j D609J interested parties. be exposed at the same time and in the same device as the Paint `j 6. Procedure 6.1 Mount the test specimens vertically both above and below the horizontal center line of the source of radiation. Rotate the specimens from the upper to lower portion ofthe test specimen. 8.4 Other methods for evaluating test specimens may be used if mutually agreed upon between all interested parties. 9. Report jj D 1005 Thiel D 1186 Dry! revolving sample rack to provide more uniform exposure conditions over their surface. Samples may also be inverted during rotation. When the exposure interval does not exceed 24 h, locate each specimen equidistant from the horizontal axis of the arc. For exposure intervals not exceeding 100 h, rotate the specimens daily. For longer exposures, expose spec imens for approximately as many hours in the top portion of the specimen rack as in the bottom portion. Other methods of achieving uniform total irradiation may be employed if 9.1 Report the following information: 9.1.1 Complete description of exposure procedure used including the following: 9.1.1.1 Light/light plus water/dark cycle used, 9.1.1.2 Operating black-panel temperature during all por tions of the exposure cycle, 9.1.1.3 Operating relative humidity, 9.1.1.4 Type and thickness of filter glass used, and 9.1.1.5 Temperature of water used for water spray. \ | i to a I . D 1212 of Oi D 1400 Dry , plied D3924 . ditior Relat mutually agreed upon between the concerned parties. 6.2 Table 1 lists test-cycle conditions commonly used for 9.1.2 Total hours of test. 9.1.3 Test specimen preparation. I TEST evaluation of paints, varnishes, lacquers, and related coat ings. As discussed in 3.1, each of the test cycles can be run 9.1.4 Identification of controls used. 9.1.5 Results of evaluation test or tests performed off Summa using different types ofglass filters. The filter glass used must specimens and control or standard samples. " 3-l A lit The American Society for Testing and.Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are entirely their own responsibility. 8,5 automa Sat and a This standard Is suP/ect to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreappraved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend, ft you feel that your comments have not received s fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 102 DUP050297285 he water iter used cified in otting. an those rimed as er spray, nine the of total uired to in either eference mens m , D 659, D2616, iuct use >rmance 1 at the ols as a lge with method ial must e as the may be parties. e used ill por- i- med on Designation: D 823 - 91 Standard Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels1 This standard is issued under the fixed designation D 323; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of iast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. These test methods have been approved jbr use by agencies of the Department cf Defense to replace Method 2121 of Federal Test Method Standard No. 141A. Consult the DoD Index ofSpecifications and Standardsfor the specific year of issue which has been adopted by the Department ofDefense. U Scope 1.1 Five test methods are given for preparing films of uniform thickness of coatings on test panels. These test methods are: Test Method A--Automatic Spray Machine Application Test Method B--Motor-Driven Dip Coater Application Test Method C--Motor-Driven Blade Film Application Test Method D--Hand-Held Spray Gun Application Test Method E--Hand-Held Blade Film Application 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory Imitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D10Q5 Test Methods for Measurement of Dry Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1212 Methods for Measurement of Wet Film Thickness of Organic Coatings2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 D 3924 Specification for Standard Environment for Con ditioning and Testing Paint, Varnish, Lacquer and Related Materials2 TEST METHOD A--AUTOMATIC SPRAY MACHINE APPLICATION 3. Summary of Test Method 3.1 A liquid material is applied to a test panel by means of an automatic spray machine consisting of a mounted spray gun and a panel holder. This machine can (i) move the 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.23 on Physical Properties of Applied Paint Films. Current edition approved Sept. 15,1991. Published November 1991. Originally published as D 823 - 45 T. Last previous edition D 823 - 87. 2 Annual Book ofASTM Standards, Vol 06.01. panel holder, with test panel, at a uniform speed through the atomized spray produced by a fixed spray gun, or (2) it can move the gun, with atomized spray, at a uniform speed past the test panel mounted on a fixed panel holder. A machine equipped.with a programmable system can index the spray gun vertically for multiple passes and for multiple coats with selective time delay. 3.2 The thickness of coating applied is controlled by the traverse speed of the panel or gun, the fluid delivery rate of the gun, the viscosity of the material, and the amount of nonvolatile matter in the material. 4. Significance and Use 4.1 This test method should be used for those coatings that are designed for spray applications of objects in the factory or in the field. It is particularly important that it be used in the evaluation of metallic coatings for appearance properties, such as gloss and color. 4.2 Coatings applied by this test method may exhibit a slight orange-peel or spray wave. 5. Apparatus 5.1 Test Panels, of any smooth, planar material of a size that can be accommodated by the panel holder of the automatic spray machine. 5.1.1 When steel panels are used, they should be prepared in accordance with the appropriate method in Methods D609. 5.2 Automatic Spray Machine,3 equipped with a panel holder and a mounting for a spray gun. The machine shall be designed to move the panel holder at a uniform speed past the fixed gun mount, or designed to move the gun mount at a uniform speed past the fixed panel holder. The panel holder or the gun mount traverse speed shall be adjustable from 25 to 100 ft (7.5 to 30 m)/min. Typical machines are shown in Fig. 1. N' I--Some automatic spray machines provide additional fea tures that can improve the uniformity of film preparation. Some examples are: a z-bar panel holder, indexing of the panel holder at right angles to the gun to provide uniform lapping; and automatic control of number of passes, time between passes, and lapping distance. 5.3 Spray Gun, any that will provide a uniform fan-type 3 Machines suitable for this purpose are manufactured by Eclipse Systems, Inc., 12 Cork Hill Rd., Franklin, NJ 07416; Spraymation, Inc., 5320 N.W. 35th Ave., Ft. Lauderdale, FL 33309-6314. 103 DUP050297286 # D 823 (b) Fixed Panel) Traveling Glm Machine the x tency NO' i wider test pa (c) Fixed Panel Programmable Indexing Traveling Gun Machine 7.3 FIG. .1 Automatic Spray Machines, Method A macl a few : spray pattern at least 6 in. (150 mm) in width is satisfactory. The gun may be triggered manually or automatically. 5.4 Pressure Gage, covering the range of 0 to 100 psi (0 to 690 kPa). 5.5 Air Pressure Regulator. 5.6 Air Supply, oil-free, under pressure. 6. Preparation of Apparatus ' 6.4 Set the automatic spray machine controls to provide the desired traverse speed of the panel holder or the gun mount, whiehever is pertinent to the type of machine being used. j : N' 3--Suitable traverse speeds for automative coatings usually range from 700 to 900 in./jnin (17.5 to 22.5 m/min). ' ._ ' | I ; and leave 7.4 air-di adus 7.5 with which 6.1 Mount the spray gun on the automatic spray machine. 7. Procedure Connect the air line hose from the regulator to the air 7.1 Strain the material to be.sprayed into the container to 8. Re pressure gage which in turn is connected to the air inlet ofthe be used with the spray gun. Reduce the material to a ji spray gun. viscosity suitable for spraying. ; 6.2 Set the gun so that its tip is at the desired distance 7.2 Connect the container to the gun and test the spray from the test panel surface, usually in the range from 8 to 12 gun operation while stationary, for correct spray pattern and 8.1 8.1. 8.1. rial, .< in. (200 to 300 mm). uniformity ,by allowing a momentary spray to be deposited I 6.3 With the gun trigger fully open, adjust the air regu- on a piece of paper placed in the panel position. Adjust the 1 8.1. ` 8.1. lator to provide the desired reading on the air pressure gage. air pressure material flow, and spray fan width controls until 1 8.1. ` N' 2- -A suitable air pressure is usually from 40 to 75 psi (275 to 520 kPa). foe desired pattern and uniformity are obtained. Further refinements may be made in the spray pattern by modifying I 8.1. ` 8.1. ` cation 104 DUPO 50297287 >vide gun >eing usually iner to 1 to a spray rn and josited jst the s until urther iifying (a) Dip-Coater Wltti Motor-Oriven Step-Cone Pulley (6) Dlp-Coater With Continuously Variable Speed Drive FIG. 2 Dip-Coaler the air pressure, the type of thinning agent, and the consis tency of the material. N' 4--The width of the spray pattern should be considerably wider than the width of the test panel to assure spray uniformity on the test panel. 7.3 Place a test panel on the panel holder and start the machine. Operate the spray gun so that it will begin spraying a few seconds before the test panel enters the spray pattern and continue spraying a few seconds after the test panel leaves the spray pattern. 7.4 Remove the coated panel and bake, force-dry, or air-dry it, in accordance with its type, in a vertical position in adust-free atmosphere, as described in Specification D 3924. 7.5 Determine the thickness of the coating in accordance with Test Methods D 1005, D 1186, D 1212, or D 1400, whichever is appropriate. 8. Report 8.1 Report the following information: 8.1.1 Type of coating material, 8.1.2 Viscosity and percent of nonvolatile coating mate rial, 8.1.3 Distance of test panel from gun tip, 8.1.4 Air pressure, 8.1.5 Number of spray passes, 8.1.6 Traverse speed; 8.1.7 Temperature and relative humidity at time of appli cation, and 8.1.8 Film thickness values obtained for applied coating. 9. Precision 9.1 The precision of preparing coated panels by this test method depends on the type of coating applied and its thickness. 9.2 For most types of coatings, individual thickness read ings taken over the surface of the applied coating can be expected to deviate from the mean by no more than 5 %. METHOD B--MOTOR-DRIVEN DIP COATER APPLICATION 10. Summary of Test Method 10.1 A motor-driven device is employed to withdraw the test panel from a container of the coating material at a desired uniform rate. 10.2 The thickness of coating applied isxontrolled by the speed of panel withdrawal, the viscosity of the material, and the percent of solids in the material. 11. Significance and Use 11.1 This test method is limited to those materials that flow oilt to smooth films When test panels are dipped into the material and withdrawn. 105 DUP050297288 # D 823 12. Apparatus 12.1 Dip Coaler,4 consisting of a mechanism that will withdraw a panel from a container ofthe coating material at a predetermined rate. Suitable apparatus, is shown in Fig. 2(a) and 2(6): 12.1.1 The apparatus shown in Fig. 2(a) uses a cord wound around a step-cone pulley on the shaft of a motor to provide panel withdrawal rate of 2, 3, and 4-in. (50, 75, and 100-mm)/min. Prior to withdrawal, the panel, attached to the cord, is lowered by hand into the container holding the material. 12.1.2 The apparatus shown in Fig. 2(0) uses a cord driven by a variable-speed device that can provide panel immersion and withdrawal rates that are continuously vari able from 2.5 to 20 in. (65 to 510 mm)/min. N' 5--Rectangular containers (F-style can with lid cut off) are useful because the smaller exposed surfaces of the liquid coating reduces volatile loss. 12.2 Test Panels, of any clean, smooth, rigid substrate ofa size that can be accommodated by the dip coater and the container. 12.2.1 When steel panels are used they shall be prepared in accordance with the appropriate method in Methods D609. N' 6--The test panels should not exceed 12 in. (300 mm) in length, but the width may be varied up to 12 in. if a suitable counterweight is used and a dip tank ofadequate size is provided. Use of a multiple hook will permit dipping several panels at one time. 13. Procedure 13.1 Adjust the coating material to the proper percentage of solids and viscosity. Measure the temperature of the material in the container at the time of application. N' 7--The operating conditions (viscosity, percent of nonvolatile matter, and rate of withdrawal) are specific for a given coating material and film thickness and need to be determined by trial. Subsequent reproduction of the same operating conditions should rive the same film thickness. Data are available5 on a variety of materials and film thickness to indicate the range required. The viscosity range for normal film thickness of0.5 to 2.0 mil (13 to 50 mm) has been shown to be 1 to 2.5 P. ^ 13.2 Place the prepared test panel on the hook attached tor the cord and lower it into the container holding the coating material. Wind the cord once completely around the pulley of the correct size to give the desired rate of withdrawal. 13.2.1 For the stepped-cone pulley apparatus, wind the cord once completely around the pulley of the correct size to give the desired weight of withdrawal. 13.2.2 For the continuously variable speed apparatus set the desired panel immersion and withdrawal rates on the control panel. 13.3 Start the motor and withdraw the panel at the desired rate, with a smooth movement entirely free of 4 Suitable dip coaters are the Garard Dip Coater obtainable from Paul N. Gardner Co., Inc., 316 N.E. First St., P.O. Box 10689, Pompano Beach, FL 33061-6688 and die Dipcoater obtainable from Technical Equipment Co., P.O. Box 208, Willoughby, OH 44094. 5 Information covering viscosity, percent of solids, rates ofwithdrawal and film, thickness for a variety of finishing materials is given in the paper by Payne, H. F., "The Dip Coater, An Instrument For Making Uniform Filmsby the Dip Method," Industrial and Engineering Chemistry, Analytical Edition, Vd IS, 1943, p. 48.' vibration. Bake, force-dry, or air-dry the coated panel, in accordance with its type, in a vertical position in a dust-free atmosphere in accordance with Specification D 3924. 13.4 Determine the thickness ofthe coating in accordance with Test Methods D 1005, D 1186, or D 1400, whichever is appropriate. 13.5 If the coating thickness is too low, coat another panel using a slower rate of panel withdrawal. If the coating thickness is too high, coat another panel using a faster rate of panel withdraw. 13.6 Continue in this manner until a test panel having the desired film thickness is produced. Measure thickness on at least three different areas of the test panel to determine coating uniformity. N' 8--With the dip coater, non-uniform thickness on a panel is frequently obtained. Hence, ifthe film thickness is greater at the bottom than the top, the viscosity should be increased or the panel withdrawal speed should be reduced, or both. 14. Report 14.1 Report the following information: 14.1.1 Type of coating material, 14.1.2 Viscosity, temperature, and percent nonvolatile of coating material, 14.1.3 Rate of withdrawal, 14.1.4 Air temperature and relative humidity at time of application, and 14.1.5 Mean and range of dry film thickness values obtained. 15. Precision 15.1 The precisian of preparing coated panels by this test method depends on the type of coating applied and its thickness. 15.2 For most types of coatings, individual thickness readings taken over the surface ofthe applied coating can be expected to deviate from the mean by no more than 5 %. METHOD C--MOTOR-DRIVEN BLADE FILM APPLICATION 16. Summary of Test Method 16.1 A uniform film is produced by an applicator blade that is pushed across the test panel at a uniform speed by a motor-driven device. 16.2 The thickness of coating applied is controlled by the clearance of the applicator blade and the viscosity and percentage of solids of the material. 17. Significance and Use 17.1 This test method is applicable to substrates consisting of smooth rigid materials, such as metal or glass, and of non-rigid materials, such as paper charts. It is more reliable for producing uniform films than is the use of hand-held draw-down applicators. 18. Apparatus 18.1 Motor-Driven Blade Film Applicator,6 consisting of* j 6 Suitable apparatus may be obtained from several supplier of paint te*W equipment. - 106 base p driving flat b) desigrn blades A mecl autom: appara 18.2 rator. 18.3 adjusta 18.4 may be N' panels si Test Me 19. Pr< DU PO 50297289 :ordance ehever is ler panel coating :r rate of iving the > on at Jtermine a panel is he bottom : vithdrawal olatile of t time of s values ' this test . and its thickness tgcanbe n 5 %. A )r blade :ed by a d by the jity and consisting s, and of :e reliable aand-held isting ofa paint testing FIG. 3 Blade Film Applicator, Motor-Driven, Method C base plate, a bar for holding an applicator blade, and a driving mechanism. The base plate shall hold paper charts Bat by means of a vacuum. The blade holder shall be designed to accommodate common types of applicator blades and to accept weights for loading the applicator blade. A mechanism shall be provided to stop the blade movement automatically at the end of the draw-down. A suitable apparatus is shown in Fig. 3. 18.2 Vacuum Source, a vacuum pump or a water aspi rator. 18.3 Applicator Blade, any common type, either with adjustable or fixed clearances. 18.4 Test Panels, any dean, smooth, rigid substrate or may be paper charts or similar materials. - . , N' 9--Rigid panels shall be cleaned in an approved manner,- Steel; panels shall be prepared in accordance with'the appropriate method in Test Method D 609. 19. Procedure ;!- 19.1 Clean the base plate and place the test panelon it: 19.2 If a vacuum is needed to hold the test panel flat, connect the vacuum source to the base plate and turn.it on. N' 10--When films are-'being applied to paper charts or tin foil, a sheet of paper should first be placed on the vacuum plate to prevent formation of dimples at the plate perforations. 19.3 Select an applicator blade having a clearancte that should provide a wet film thickness that wifi give the desired dry film thickness; or, if specified; the required wet film thickness. Insert the blade in the blade holder and load the holder with weights if needed. 19.4 Place a suitable amount of the coating material on the test panel in front ofthe blade. Start the motor-drive and teat the test panel. :l .*9.5 Remove the coated panel and bake, force-dryor jttf'dry the coating, in' accordance with its type, in a tXjnzontal position in a dust-free atmosphere in accordance Wlth Specification D 3924. N' 11--Paper charts should be taped down to prevent curling of the edges that causes the wet film to flow towards the center. 19.6 Clean the applicator blade. 19.7 Determine the thickness of the applied coating in accordance with Test Method D 1005, D 1186, or D 1400 whichever is appropriate. 19.8 Ifthe coating thickness is too low, coat another panel using a larger blade clearance. If the coating thickness is too high, coat another panel using a smaller blade clearance. 19.9 Continue in this manner until a test panel having the desired dry film thickness is produced. Measure thickness on at least three different areas of the test panel to determine coating uniformity. - 20. Report 20.1 Report the following information: 20. t.'l Type of coating- material, - 20.1.2 Viscosity and percentage of solids of coating mate rial; 20.1.3 Clearance of applicator blade used, 20.1.4 Air temperature and relative humidity at time of application, and 20.T.5 Mean and range of the film thickness values obtained. 21. Precision 21.1 The precision of preparing coated panels by this test method depends on the type of coating apphed and 'its thickness.' r 21.2 For most types of coatings; individual thickness readings taken over the surface ofthe apphed coating can be expected to deviate no more than 5 % from the mean. METHOD D--HAND-HELD SPRAY GUN APPLICATION 22. Summary of Test Method 22.1. -A uniform film of a coating material is produced on 10? DUP050297290 D823 a test panel by the means of a spray gun hand-held by a person skilled in its use. 22.2 The thickness of coating applied is controlled by the traverse speed of the gun, the number of passes of the gun, the fluid delivery rate of the gun, the viscosity of the fflatwial, and the amount of nonvolatile matter in the material. 23. Significance and Use 23.1 This test method is applicable to the coating of substrates consisting of smooth, rigid materials, such as metal or glass. It is usually less reliable for producing uniform films than is the automatic spray method. However, films sufficiently uniform for most physical property tests of materials can be produced by a hand-heldspray gun oper ated by a person skilled in its use. 24. Apparatus 24.1 Spray Gun, any that will provide a uniform fan-type spray pattern at least 6 in. (150 mm) in width is satisfactory. 24.2 Air Pressure Gage, covering the range from 0 to 100 psi (0 to 690 kPa). 24.3 Air Pressure Regulator. 24.4 Air Supply, oil-free and under pressure. 24.5 Panel Holder. 25. Preparation of Apparatus 25.1 Connect the air line hose from the regulator to the air pressure gage which in turn is connected to the air inlet of the spray gun. 25.2 With the trigger fully open, adjust the air regulator to provide the desired reading on the air pressure gage. N' 12--A suitable air pressure is usually from 40 to 75 psi (275 to 520 kPa). 26. Procedure 26.1 Strain the material to be sprayed into the container to be used with the spray gun. Reduce the material to a viscosity suitable for spraying. 26.2 Connect the container to the gun and test the spray gun operation for correct spray pattern and uniformity by allowing a momentary spray to be deposited on a piece of paper placed in the panel position. Adjust the air pressure?, material flow, and spray width controls until the desired pattern and uniformity are obtained. Further refinements may be made in the spray pattern by modifying the air pressure, the type of thinning agent, and the consistency of the material. N' 13--The width of the spray pattern should be considerably wider than the width of the test panel to assure spray uniformity on the test panel. 26.3 Place a test panel on the panel holder. Hold the spray gun tip 10 to 12 in. (250 to 300 mm) from the test panel surface and trigger the spray gun. Begin by aiming the gun at right angles to the panel so that the spray pattern is just beyond the edge of the panel. Gradually make the spray pattern move across the panel at a traverse speed of 10 to 15 in. (250 to 400 mm)/s. 26.4 Reverse the traverse direction of the spray gun and make the spray pattern move across the panel again. 26.5 Remove the panel from its holder and bake or air-dry the coating, in accordance with its type, in a horizontal position in a dust-free atmosphere in accordance with Specification D 3924. 26.6 Clean the spray gun with solvent. 26.7 Measure the film thickness ofthe dry applied coating in accordance with Test Methods D 1005, D 1186, or D 1400 whichever is appropriate. 26.8 Ifthe coating thickness is too low, coat another panel using more passes of the spray pattern. If the coating thickness is too high, coat another panel with fewer passes of the spray pattern or, ifthis is not feasible, reduce the material further with thinner. | 27. Report 27.1 Report the following information: 27.1.1 Type of coating material, 27.1.2 Viscosity and percent nonvolatile of coating mate rial, 27.1.3 Temperature and relative humidity at time of application, and -"27.1.4 Mean and range of dry film thickness values obtained. 28. Precision 28.1 The precision of preparing coated panels by this test method depends on the type of coaling applied, and its thickness and the skill of the operator. 28.2 For most types of coatings, individual thickness readings taken over the surface of the applied coating can be expected to deviate from the mean by no more than 10 % if the coating has been applied by a skilled operator. METHOD E--HAND-HELD BLADE FILM APPLICATION 29. Summary of Test Method 29.1 A uniform film of a coating material is produced on a test panel by the means of a hand-held applicator blade. 29.2 The thickness of coating applied is controlled by the rate at which the applicator blade is drawn across the test panel, the viscosity of the material, the amount of nonvola tile matter in the material, and the clearance of the blade. I I f \ ` !: >. i ' ; f 30. Significance and Use 30.1 This test method is applicable to the coating of substrates consisting of smooth, rigid materials such as metal or glass. It is applicable to the coating of smooth cardboard and paper charts if some means is used to assure that these substrates are held flat. 30.2 This test method is usually less reliable for producing uniform films than is the motor-driven applicator blade method. However, films sufficiently uniform for most phys ical property tests of materials can be produced by a hand-held applicator blade operated by a person skilled in its use. f ( [ 31. Apparatus.- , 31.1 Film Applicator Blade, any common type, either with adjustable or fixed clearances. 31.2 Auxiliary Flattening Bar, precision ground.' 31.3 Test Panels, any clean, smooth, rigid substrates or may be paper charts or other similar materials. 32. P: 32.1 will pi desirec 32.2 32.2 panel. 32.2 and pi (2501< 32.3 32.3 panel; Place t Fig. 4) 32.3 and pa (250 t< applies advanc 32.4 with ii sphere 32.5 32.6 in acc D HOC 108 DUP050297291 in a dance oating <6, or panel oating ssesof aterial mate- me of values bis test md its ickness can be 10% if t on iced on ilade. by the the test involaade. ing of metal iboard at these oducing >r blade st physd by a ed in its PRIMARY APPLICATOR PAINT 823 > DIRECTION OF DRAWDOWN AUXILIARY FLATTENING 8AR > CHART GLASS PLATE-FLAT-1/4 in.(06.4 mm) THICK FIG. 4 Use of Auxiliary Flattening Bar 32. Procedure 32.1 Select an applicator blade that has a clearance that will provide a wet film thickness that should result in % desired film thickness. 32.2 For coating rigid substrates: 32.2.1 Position the applicator blade near the edge of the panel and place a pool of the liquid material in front of it. 32.2.2 Grasp the sides of the applicator with the fingers and pull it across the panel at a speed of about 10 to 12 in. (250 to 300 mm)/s. 32.3 For coating non-rigid substrates: 32.3.1 Position the applicator blade near the edge of the panri and place a pool of the liquid material in front of it. Place the auxiliary bar in front of the pool of material (see fig-4). 32.3.2 Grasp the sides of the applicator with the fingers and pull it across the panel at a speed of about 10 to 20 in. (250 to 500 mm)/s. As the auxiliary bar is pushed by the applicator, it should press the substrate flat adjacent to the advancing edge of the applicator. 32.4 Bake or air-dry the applied coating, in accordance with its type in a horizontal position in a dust free atmo sphere in accordance with Specification D 3924. 32.5 Clean the applicator bar with solvent. 32.6 Measure the film thickness ofthe dry-applied coating in accordance with Test Methods D 1005, D1186, or D1400 whichever is appropriate. 32.7 If the coating thickness is too low, select an appli cator blade with a greater clearance and coat another panel. If the coating thickness is too high, select an applicator blade with a smaller clearance and coat another panel. 33. Report 33.1 Report the following information: 33.1.1 Type of coating material, 33.1.2 Viscosity and percent nonvolatile of coating mate rial, 33.1.3 Clearance of applicator blade used, 33.1.4 Air temperature and relative humidity at time of application, and 33.1.5 Mean and range of the film thickness values obtained. 34. Precision 34.1 The precision of preparing coated panels by this test method depends on the type of coating applied, its thickness and the skill of the operator. 34.2 For most types of coatings, individual thickness readings taken over the surface of the applied coating can be expected to deviate from the mean by no more than 10 % if the coating has been applied by a skilled operator. 35. Keywords 35.1 automatic spray; blade applicator; dip coater; organic coatings The American Society for Testing and Materials takes no position respecting the validity at any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive carelul consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. either 109 DUP050297292 4 Designation: D 868 - 85 (Reapproved 1989)1 Standard Test Method for Evaluating Degree of Bleeding of Traffic Paint1 This standard is issued under the fixed designation D 868; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. ei N' --Editorial changes were made throughout, including the tide, in October 1989. 1. Scope 1.1 The photographic reference standards that are part of this test method2 are representative ofthe degrees ofbleeding of traffic or pavement marking paints. The standards are intended primarily for comparative evaluation in the labora tory. 1.2 Bleeding as defined is the only type ofdiscoloration in this test method. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standard: D969 Test Method for Laboratory Determination of Degree of Bleeding of Traffic Paint3 2.2 Adjunct: D 868 Bleeding resistance of paint (one photo)2 3. Terminology 3.1 Description of Term Specific to This Standard: 3.1.1 bleeding characteristic--that condition of discolora tion manifested in traffic paint when applied to tar or asphaltic-type substrates. The number assigned to evaluate the degree of bleeding failure represents in these reference standards a measure of the contrast between the color of the 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.44 on Traffic Coatings. Current edition approved Nov. 29, 1985. Published January 1986. Originally published as D 868 - 46 T. Last previous edition D 868-48 (1981)*1. 2 Copies of the pictorial photographic reference standards are contained in the publication Pictorial Standards of Coating Defects, and may be obtained from ASTM Headquarters (request Adjunct PCN 12-408680-00) or the Federation of Societies for Coating Technology, 492 Norristown Rd., Blue Bell, PA 19422. The original source of the photographic reference standards illustrated in Fig. I is the Federation. 2 Annual Book ofASTM Standards, Vol. 06.01. dry film on a nonbleeding surface and the color of the dry film on the test surface. 4. Significance and Use 4.1 Solvents in a traffic paint may cause bleeding of pavement constituents into the traffic marking, thereby rendering the traffic marking less effective as a lane or directional indicator. This test method in conjunction with the method for panel preparation in Test Method D 969 is used to evaluate such bleeding properties. The evaluation is very subjective and raises questions as to the usefulness of the results for specification compliance. 5. Use of Photographic Reference Standards 5.1 The photographic reference standards that are part of this test method2 are representative of the degrees of bleeding of traffic or pavement marking paints. The photograph in Fig. 1 is for illustration purposes only and should not be used for evaluation. 5.2 The use of the photographic reference standards shown in Fig. 1 should be as follows: 5.3 In preparing films to compare with the reference standards for evaluating the extent of bleeding, the paint shall be applied to: 5.3.1 A nonbleeding reference surface, and 5.3.2 The test surface. 5.4 The paint under test shall be applied at a film thickness sufficient to ensure complete hiding. 5.5 The contrast in color between the films over the nonbleeding reference surface and the test surface shall be compared with the reference standards in Fig. 1 for a numerical rating. N' --The degree of bleeding must necessarily be a function ofboth : the bleeding surface agreed upon and the initial color of the paint For instance, a yellow paint in general would be expected to show less bleeding than a white paint since its initial color is darker and as a consequence the discoloration effect of the bleeding surface upon this I darker color will be minimized. i 6. Precision and Bias I 6.1 Precision--Due to the poor precision of this test I method, if it is used in a specification, the permissible I deviation from the maximum specified value should be I agreed upon between die purchaser and the seller. 1 6.2 Bias--Bias cannot be determined. I 110 DUPO 50297293 r of the dry bleeding 0f ng, thereby i a lane or inction with od D 969 is valuation is isefulness of t are part of 5 of bleeding otograph in i not be used e standards ie reference g, the paint 1 at a film is over the tee shall be ig. 1 for a action of both the paint. For i to show less irker and as a face upon this of this test permissible e should be er. D868 TRAPFiC PAINT COLOR. BLEEDING STANDARDS FIG. 1 Degrees of Bleeding The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1S16 Race St., Philadelphia, PA 19103. Ill DUP050297294 A 4111 Designation: D 869 - 85 (Reapproved 1989)61 Standard Test Method for Evaluating Degree of Settling of Paint41 1 This standard is issued under the fixed designation D 869; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of hist teapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This method has been approved for use by agencies of the Department of Defense to replace Method 4208 of Federal Test Method Standard No. 141A Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 41 N' --Editorial changes were made throughout, including the title, in October 1989. l Rating 0 6. Pr< 6.1 1. Scope 1.1 This test method covers the determination of the degree of pigment suspension and ease of remixing a shelf-aged sample of paint to a homogeneous condition suitable for the intended use. 1.2 This standard may involve hazardous materials, oper ations and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D1309 Test Method for Settling Properties of Traffic Paints During Storage2 3. Significance and Use 3.1 Paints, if not formulated or processed properly may settle excessively. Paint that settles excessively is difficult to reincorporate into the paint system causing time delays or valuable pigment being left in the drum. This test method is an attempt to evaluate the degree of settling caused by the accelerated Test Method D1309. This very subjective method of evaluation in conjunction with the variables of Test Method D 1309 raises questions as to the usefulness of the results for specification compliance. 4. Apparatus 4.1 Container, standard 1-pt (500-mL) friction-top can paint container, 3% '/i6 in. (85.5 1.5 mm) in diameter, and 3% Vu in. (98.5 1.5 mm) in height 4.2 Spatula, weighing 45 1 g with square-end blade 4% in. (125 mm) in length and approximately 13/i6 in. (20 mm) in width, shall be used to examine the paint for pigment settling and reincorporation characteristics. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.44 on Traffic Coatings. Current edition approved Sept. 27, 1985. Published November 1985. Originally published as D 869 - 46 T. Last previous edition D 869 - 78. 2 Annual Book ofASTM Standards, Vol 06.01. 5. Procedure 5.1 Place the specimen to be tested for pigment suspen sion in a 1-pt (500-mL) container, filling the can to within lh in. (13 mm) of the top. Gose the can tightly and hold undisturbed for shelf aging for 6 months or for such other periods of time agreed upon between the purchaser and the seller. 5.2 Open the can holding the shelf-aged sample without shaking or agitation, and examine the sample without removal of supernatant vehicle. Use the spatula to determine the extent and character of portions of the paint that may have separated during storage. Prepare a suitable spatula for this purpose by cutting the tip from an ordinary 5-in. (127-mm) flexible steel laboratory spatula to the specified length. Hold the spatula perpendicular to and in the center area of the paint at a height whereby the bottom edge of the spatula is level with the top of the can. Drop the spatula from that position. Rate the condition of the sample in accordance with 5.4. 5.3 After examination of the entire specimen as described in 5.2, if a portion of the pigment has separated out to form a firm cake at the bottom of the container pour the supernatant portion of the liquid off into a clean container and hold for subsequent use. Reincorporate the separate cake by hand stirring with the spatula, adding back the liquid in small amounts until the pigment has been reincorporated to form a homogeneous paint suitable for the intended use or until it is determined that the pigment cake cannot be reincorporated by hand stirring. Rate the condition of the specimen in accordance with 5.4. 5.4 Rate the sample for degree of settling on a scale from 10 to 0 in accordance with the following. Give intermediate conditions the appropriate odd number. Rating Description of Paint Condition 10 Perfect suspension. No change from the original condition of the paint. 8 A definite feel ofsettling and a slight deposit brought up on spatula. No significant resistance to sidewise movement of spatula. 6 Definite cake ofsettled pigment Spatula drops through cake to bottom of container under its own weight Definite resistance to sidewise motion of spatula. Coherent portions of cake may be removed on spatula. 4 Spatula does not fall to bottom of container under its own weight. Difficult to move spatula through cake sidewise and slight edgewise resistance. Paint can be remixed readily to a homogeneous state. 2 When spatula has been forced through the settled layer it is very difficult to move spatula sidewise. Definite edgewise resistance to movement of spatula. Paint can be remixed to a homogeneous state. 112 r r k. k. I k. DUP0502 97295 D 869 Rating Description of Paint Condition 0 Very firm cake that cannot be reincorporated with the liquid to fotm a smooth paint by stirring manually. 6. Precision and Bias 6.1 Precision--Due to the poor precision of this test method, if it is used in a specification, the maximum deviation from the settling limits specified should be agreed upon between the purchaser and the seller. 6.2 Bias--Bias cannot be determined. f The American Society lor Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection \ with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement oI such rights, are entirely their own responsibly. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and II not revised, eitherreapproved or withdrawn. Your comments are Invited either forrevision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. II you teal that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. pnent suspenin to within l/i ltly and hold or such other baser and the .mple without nple without i to determine aint that may yle spatula for irdinary 5-in. the specified in the center m edge of the : spatula from in accordance i as described d out .to form ler pour the san container separate cake the liquid in orporated to ended use or ; cannot be iition of the i a scale from intermediate Iition of the paint up on spatula. No tula. gh cake to bottom stance to sidewise iv be removed on r its own weight, nd slight edgewise ngeneous state, i layer it is very wise resistance to jmogeneous state. DU P0502 97296 <1 Designation: D 870 - 87 Standard Practice for Testing Water Resistance of Coatings Using Water Immersion1 This standard is issued under the fixed designation D 870; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapprovai. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice covers the basic principles and' operating procedures for testing water resistance of coatings by the partial or complete immersion of coated specimens in distilled or de-mineralized water at ambient or elevated temperatures. Although the apparatus and procedure could be employed in immersion tests using solutions of various materials in water, this practice is limited to tests in water alone. 1.2 This practice is limited to. the methods of obtaining, measuring, and controlling the conditions and procedures of water immersion tests. It does not specify specimen prepara tion, specific test conditions, or evaluation of results. N' 1--Alternative practices for testing the water resistance of coatings include Practices D 1735, D 2247, and D 4585. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. .2. Referenced Documents 2.1 ASTM Standards: D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products12 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces2 D714 Test Method for Evaluating Degree of Blistering of Paints2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, Lacquer, and Related Products on Test Panels2 D1193 Specification for Reagent Water3 D1730 Practices for Preparation of Aluminum and Aluminum-AUoy Surfaces for Painting4 D 1735 Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus2 D 2247 Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity2 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO1.27 on Accelerated Testing. Current edition approved Nov. 27, 1987. Published January 1988. Originally published as D 870 - 46 T. Last previous edition D 870 - 86a. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.05 and 11.01. 4 Annual Book ofASTM Standards, Vols 02.05 and 06.01. D2616 Test Method for Evaluation of Visual Color Difference with a Gray Scale5 D3359 Test Methods for Measuring Adhesion by Tape Test2 D3363 Test Method for Film Hardness by Pencil Test2 D4585 Practice for Testing Water Resistance of Coatings Using Controlled Condensation2 3. Summary of Practice 3.1 Coated specimens are partially or wholly immersed in water in a container that is resistant to corrosion. The exposure conditions are varied by selecting: (a) the tempera ture of the water, and [b) the duration of the test. Water permeates the coating at rates that are dependent upon the characteristics of the coating and upon the temperature of the water. Any effects such as color change, blistering, loss of adhesion, softening, or embrittlement are observed and reported. 4. Significance and Use 4.1 Immersion in water can cause the degradation of | coatings. Knowledge on how a coating resists water immer sion is helpful in predicting its service life. Failure in a water immersion test may be caused by a number of factors including a deficiency in the coating itself, contamination of the substrate, or inadequate surface preparation. The test is therefore useful for evaluating coatings alone or complete coating systems. 4.2 Water immersion tests are used for research and development of coatings and substrate treatments, specifica tion acceptance, and quality control in manufacturing. These tests typically result in a pass or fail determination, but the degree of failure may also be measured. A coating system is considered to pass if there is no evidence of water-related failure after a specified period of time. 4.3 Results obtained from water immersion tests in accor dance with this practice should not be represented as being equivalent to a period of exposure to water in the natural environment, until the degree of quantitative correlation has been established for the coating or coating system. 4.4 Corrosion tests of a scribed coating on a ferrous substrate are impractical in water immersion tests as the corrosion products tend to contaminate the water bath | Continuous overflow of the test tank is sometimes required | to maintain consistent water quality. 4.5 The apparatus for the test is relatively inexpensive and] can be as simple as a glass beaker with a stirrer. It is 5 Annual Book ofASTM Standards. Vol 14.02. 114 P o H o ai cc 3< Wl OH 6. sp tic sb sul M< un 7. spe the Spi cin fie< ten of i Prc DU FO50297297 D 870 of A f Visual Co!0r hesion by Tape y Pencil Test* lDce of Coatinj, )Uy immersed in corrosion. The (a) the temper*, the test. Water indent upon the : temperature of blistering, loss of e observed and : degradation of sts water immer ailure in a water imber of facton contamination of ation. The test is one or complete Dr research and ments, specific* ifacturing. These lination, but the mating system is of water-related ;ion tests in accor^resented as beint ter in the natural ive correlation ins ; system, ing on a ferrous irsion tests as the > the water banDmetimes require 4rttiaraWs 5. r u constructed of corrosion-resistant materials. 5.1 ^iiits, if required, should preferably be located > >-' . tank. Oats>oe for circulation of the water with pressurized ^cftrer or a pump. *iui<iuovorts for the Test Specimens, constructed of non- 5-3 jrive materials to hold the specimens 30 mm apart and from the bottom and sidewalls of the tank. & ^ . n,e circulating system is for the purpose ofexposing all the tf^rhetank t0 mom air so the water does not become stratified and **^epleted at the lower levels. , Test Specimens * jhis practice does not cover the preparation of test J^Liens. The substrate composition and surface prepara- eCflmecimen preparation, and the number of specimens jjjUlldbeagreed upon prior to testing. - 3--Applicable methods for the preparation of test panels and iL-rttes a** 6'ven in Mettl<xl ^ 609 and Practice D 1730. Test Jjjjjjods D823 covers application techniques for the production of; jjjionn fil1115- 7. Procedure 71 Fill the tank with water to a depth where the test ^msns are immersed for approximately three-quarters of Ibdr length. Reagent water conforming to Type IV of Specification D 1193 is suitable for use. . 12 Hmt the water to the desired temperature with the glaring system in operation. If no temperature is speci fied, heat the water to 100 2F (38 1"C). Maintain the temperature throughout the test. 7.3 Place the test specimens in the tank so that the plane of the specimens is parallel to the flow of water in the tank: Protect the edges and backs of the specimens from corrosion if these surfaces are not to be tested. 7.4 Replace the water if it becomes cloudy or colored. Continuous replacement of the water is permitted. 7.5 Conclude the test after a specified period of time or after effects from water immersion have been observed. 7.6 Wipe the test specimens dry. Rate specimens for changes in color, blistering, etc. Evaluate specimens no less than 5 min and no more than 10 min after removal from test, as the effects from water exposure can change within a short time. Remove only as many specimens as can be rated within the specified time. N' '4--The 0 to 10 scale described in ASTM STP 5006 is preferred for rating. Relevant procedures for evaluating water effects are described in Test Methods D 610, D 714, D 2616, D 3359, and D 3363. 7.6.1 If possible, rate the specimens again after they have been removed from the test for a recovery period long enough that moisture absorbed within the specimens dries out and the specimens reach moisture equilibrium with room air. A recovery period from 12 to 24 h is generally sufficient. The post-recovery rating allows evaluation of the permanent effects of the exposure as distinct from the transient effects, and is especially important for evaluation of color and gloss. 8. Report 8.1 Report the following information: 8.1.1 Sample identification. 8.1.2 Results of the evaluations). 8.1.3 Reference to Practice D 870. 8.1.4 Hours of test duration. 8.1.5 Test temperature. 8.1.6 Brief description of water quality and water replace ment procedure. 8.1.7 Special conditions of test or any deviations in test procedure. 6 Paint Testing Manual, ASTM STP 500, ASTM, 1972. The American Society for Testing end Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by tlfe responsible technical committee end must be reviewed every live years and it nth revised, eitherreapproved or withdrawn. Your comments are Invitedeither forrevision ofthis standardor foradditional standards and should be addressed to ASTM Headquarters. Your comments wUI receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to she ASTM Committee on Standards, 1916 flace St., Philadelphia, PA 19103. ly inexpensive a a stirrer. It is s* 115 DUP050297298 IT' <1 Designation: D 913 - 88 Standard Test Method for Evaluating Degree of Resistance to Wear of Traffic Paint1 This standard is issued under the fixed designation D 913; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapptoval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the evaluation of degree of resistance to wear that may occur with traffic paints in road tests (see Practice D 713) or in actual service, using photo graphic standards for comparative evaluation. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D713 Practice for Conducting Road Service Tests on Fluid Traffic Marking Materials2 3. Description of Term Specific to This Standard 3.1 failure, described by these reference standards--that condition manifested in traffic paint by actual detachment of entire sections of the film from its substrate or from paint previously applied. The degree of resistance to failure is judged by the amount of substrate that is covered. 5. Type of Failure 5.1 The failure as described in Section 3 does not presume any specific mechanism, and all areas where the substrate is visible shall be considered a failure. 6. Use of Photographic Reference Standards 6.1 The photographic reference standards3 that are part of this test method are representative of the degrees of resist ance to wear of stripes of traffic paint. The examples shown in Fig. 1- are for illustration purposes only and should not be used for evaluation. 6.1.1 The degree of resistance to wear is likely to vary over any given area. It is therefore necessary to use one of the following grading methods: 6.1.1.1 Select an area as representative and base the rating of the stripe on this area or 6.1.1.2 Grade segments of the stripe and average these gradings. 6.1.2 The photographic reference standards (Note) repre sent four degrees (97 %, 92 %, 77 %, 60 %) of resistance to wear. Substrate revealed by failure is readily discernible with the naked eye. N' --The reference standards are representative ofstripes of traffic paints. The percentage of surface covered is shown on each reference standard. 4 Significance and Use 4.1 This test method is designed to evaluate the resistance to wear of a traffic paint. It must be remembered that a high degree of performance ofpaint applied to a bare road surface may not guarantee similar results when the same paint is applied over old paint lines. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.44 on Traffic Coatings. Current edition approved March 23, 1988. Published May 1988. Originally published as D 913 - 47 T. Last previous edition D 913 - 83. 2 Annual Book ofASTM Standards. Vot 06.01. 7. Procedure '7.1 Compare the representative areas of the traffic paint stripes with the photographic reference standards and esti mate the percent of intact film. 8. Report 8.1 Report the mean and range of the substrate coverage estimations, if appropriate. 3 Full-size (8 by 10-in. (203 by 254-mm)) glossy prints of the photograpliit reference standards showing degrees of chipping are available from ASTM Headquarters. Order PCN 12-409130-00. i The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any suoh patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthia standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Baca St., Philadelphia, PA 19103. I I f ! : 116 DUP050297299 s not presume ie substrate is hat are part of rees of resist. I imples shown ; should not be y to vary over se one of the >ase the rating average these (Note) repre' resistance to icemible with stripes oftraffic i each reference : traffic paint rds and esti- ate coverage (Film 97 % Intact) t 1 92 % IMact) i t J DUP050297300 Designation: D 968 - 81 (Reapproved 1991)*1 Standard Test Methods for Abrasion Resistance of Organic Coatings by Failing Abrasive1 This standard is issued under the fixed designation D 968; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. These test methods have been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue that has been adopted by the Department ofDefense. il N' --Keywords were added editorially in January 1991. 1. Scope 1.1 These test methods cover the determination of the resistance of organic coatings to abrasion produced by abrasive Ming onto coatings applied to a plane rigid surface, such as a metal or glass panel. 1.2 Two test methods based on different abrasives are- covered as follows: Sections Method A--Falling Sand Abrasion Test Method B--Falling Silicon Carbide Abrasion Test 1-12 13-19 1.3 These methods should be restricted to testing in only one laboratory when numerical values are used because of the poor reproducibility of lie methods {see 13.1.2 and 21.1.2). Interlaboratory agreement is improved significantly when ranking is used in place of numerical values. 1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Method for Measurement ofDry-Film Thick ness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 E 11 Specification for Wire-Cloth Sieves for Testing Purposes3 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D0J.23 on Physical Properties of Applied Paint Films. Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 968 - 48 T. Last previous edition D 968 - 51 (1972). 2 Annual Book ofASTM Standards, Vol 06.01. 2 Annual Book ofASTM Standards, Vol 14.02. 3. Terminology 3.1 Description of Term Specific to This Standard: 3.1.1 abrasion resistance--the amount of abrasive re quired to wear through a unit film thickness of the coating. 4. Summary of Test Methods 4.1 Abrasive is allowed to fall from a specified height through a guide tube onto a coated panel until the substrate becomes visible. The amount of abrasive per unit film thickness is reported as the abrasion resistance of the coating on the panel. Silica sand or silicon carbide may be used, as specified. 5. Significance and Use 1 5.1 Silica sand produces a slower rate of abrasion for f organic coatings than provided by silicon carbide but, for : some types of coatings, it provides greater discrimination. 5.2 The abrasion resistance scales produced by the two methods differ, but the methods provide approximately the 1 same rankings of coatings for abrasion resistance. ! 5.3 Each of the methods has been found useful for rating j the abrasion resistance of specific types of coatings. For f example Method A (Ming sand) has been used for rating ; floor coatings while Method B (falling silicon carbide) has ! been used for rating coatings for ship decks. 6. Pete Unii than (850 No. sand exce desc METHOD A--FALLING SAND ABRASION TEST* 6. Apparatus and Materials . 6.1 Abrasion Tester, as illustrated in Figs. 1 and 2.i5l A4 gale for starting the flow of abrasive is located near the top oftheg guide tube. It consists of a metal disk inserted into a slit it the side of the guide tube with a collar covering the slit. The guide tube shall be firmly supported in a vertical posita over a suitable receptacle, which shall contain a support fa _ holding the coated panel at an angle of 45 to the vertical, si | that the opening of the tube is directly above the area to lx abraded and the distance from the tube to the coated surfas face at the nearest point is 1 in. (25 mm) when measured it | the vertical direction. The base of the apparatus shall )* fitted with adjusting screws for properly aligning the eqt ment. iI N> SOUR requi chase 7. T 7.j a pla a mi 7.: hum: chase No Methr No 4 Hipkins, C. C., and Phain, R. J., "The Falling Sand Abrasion Tester," Bulletin, No. 143, December 1946, pp. 18-22. 5 A suitable abrasion tester may be obtained from Gardner/BYK.-Gardner, Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. US DUP050297301 0968 accordance with Test Methods D 1005, D 1400 or D 1186. d: asive recoating, 2d height substrate unit film ie coating i used, as asion for a but, for (nation, y the two nately foe for rating tings. For for rating rbide) has ST4 FIG. 1 Apparatus for Falling Sand Abrasion Test 62 Standard Abrasive--Natural silica sand from the St. Peters or Jordan sandstone deposits (located in the central United States) shall be considered standard when not more than 15 % of die grains in a sample are retained on a No. 20 (850 pm) sieve and not more than 5% of the grains pass a No. 30 (600 pm) sieve after 5 min of continuous sieving. The sand is characterized by its roundness of grains and its txceptionally high silicon dioxide content. Use the sieves described in Specification Ell'. N' 1--The. abrading qualities of sand obtained from different sources may differ slightly, even though the sand meets the sieve leqmrements. Therefore, for maximum precision of test results, pur chaser and seller should use sand from the same source.6 I Test Specimens 7.1 Apply uniform coatings of the material to be tested to plane, rigid surface such as a metal or glass panel. Prepare minimum of two coated panels for the material. 7.2 Cure the coated panels under the conditions of and temperature agreed upon between the purseller. N' 2--The coatings should be applied in accordance with Test "`'tads D 823, or as agreed upon between the purchaser and the seller. N' 3--The thickness of the dry coatings should be measured in 8. Standardization 8.1 Pour a quantity of standard sand into the funnel. Examine the sand stream falling from the lower end of the guide tube and align the apparatus by means of the adjusting screws in the base until the inner concentrated core of the sand stream falls in the center of the flow when viewed at two positions at 90 to each other. Introduce a measured volume of sand (2000 10 mL is a convenient amount) and determine the time of efflux. The rate of flow shall be 2 L of sand in 21 to 23.5 s. 8.2 Secure a trial panel in the testing position, as described in 6.1, and introduce the sand in increments until a spot %2 in. (4 mm) in diameter is worn through to the base material. The overall abraded area shall be elliptical in shape, about 1 in. (25 mm) in width and IV* in. (30 mm) in length. The center of the "area of maximum abrasion shall be on the centfer line through the longer axis ofthe abraded pattern and within 9/ie to "/is in. (14 to 17 mm) of the top edge. Slight final adjustment ofthe instrument may be required to center the abrasion spot in the pattern. A final check on alignment is made by determining the amount of sand that passes through a 3/32-in. (4-mm) hole in a metal panel placed directly under the tube. Place a container under the hole in the panel and allow a weighed amount of sand to pass through the tube onto the panel. Weigh the amount of sand that passed through the hole into the container. The appa ratus can be considered to be in calibration if the amount of sand that passed through the hole is 90 to 93 % of the LOWER END OF . FUNNEL TO BE A CYLINDRICAL COLLAR FITTING SNUGLY OVER OUT'SIOE OF GUIOE TUBE UPPER END OF GUIDE TUBE AT MINIMUM DIAMETER OF FUNNEL BOTH ENOS OF GUIDE TUBE CUT SQUARE AND ALL BURRS REMOVED Tester, 'AST# ^.Gardner. I04* of acceptable sand are the Ottawa Silica Co., P.O. Box 577, Ottawa, "0; the Quackenbush Co., 3 West College Dr., Arlington Heights, U. 60004; . 164 Unimin Corp.. 50 Locust Ave., New Canaan, CT. 06841). . FIG. 2 Design Details of Abrasion Test Apparatus 119 DUP050297302 D 968 amount of sand that impinged on the panel. 12.1.3 Litres of abrasive used for each area tested, 12.1.4 Coating thickness in mils for each area tested, i1 9. Conditioning 9.1 Unless otherwise agreed upon between purchaser and 12.1.5 Abrasion resistance values for each area tested, 12.1.6 Mean abrasion resistance for each coated panel seller, condition the coated test panels for at least 24 h at 23 tested, and + 2"C and 50 5 % relative humidity. Conduct the test in 12.1.7 Mean abrasion resistance and range of the replicate the same environment or immediately on removal. coated panels. given : 16.1 16.1 duced volumi 17. Co 10. Procedure 10.1 Mark off on each coated panel three circular areas, oarh approximately 1 in. (25 mm) in diameter, and so arranged that each can be properly positioned in the panel support of the abrasion tester. Measure the thickness of the coating by Test Methods D 1005, D 1186, or D 1400 in at least three locations in each area. Record the mean of each set of measurements as the thickness of the coating over the respective area. 10.2 After conditioning, secure the coated panel in the tester as described in 6.1. Adjust the panel so that one of the marked areas will be centered under the guide tube. Pour standard sand, measured voiumetrically, into the funnel. Withdraw the gate and allow the sand to flow through the guide tube and impinge on the coated panel. Collect the sand in a container located at the bottom of the tester. Repeat this operation until a %2-m. (4-mm) diameter area of the coating has worn through to the substrate. A convenient increment of sand to employ during the test is 2000 10 mL. As the end-point is approached, increments of 200 2 mL may be introduced into the funnel. 13. Precision7 13.1 On the basis of an interlaboratory test of this test method in which three laboratories tested four types of coatings differing in their abrasion resistance, the withinlaboratory coefficient of variation was found to be 9 % with 22 degrees of freedom and the between-laboratories coeffi cient of variation 35 % with 7 degrees of freedom. Based on these coefficients, the following criteria should be used for judging the' acceptability of results at the 95 % confidence level. 13.1.1 Repeatability--Two results, each the mean ofthree runs, obtained by the same operator should be considered suspect ifthey differ by more than 25 % oftheir mean value. 13.1.2 Reproducibility--Two results, each the mean of three runs, obtained by operators in different laboratories should be considered suspect if they differ by more than 118% of their mean value. N' 7--The reproducibility of this test is improved substantially when rankings of the coatings by magnitude of abrasion resistance ate used. In the interlaboratory test for evaluating precision, ail laboratories ranked the coatings in the same order. 17.1 and sei 2Ca same e: 18. Prc 18.1 dures gi 18.2 10.2 an mine th the end 18.3 coated j 19. Calr 19.1 1 abrasion in 10.11 per mil i N' 4--When the gate is withdrawn from the guide tube, make certain that a collar covers the slit opening in the tube. METHOD B--FALLING SILICON CARBIDE TEST where: W = we 14. Apparatus and Materials T = thi 10.3 Abrade each of the remaining marked-off areas of the coated panel as outlined in 9.2. 14.1 Abrasion Tester, as described in 6.1, with two excep tions: 19.2 C ! N' 5--Check the alignment of the guide tube at frequent intervals 14.1.1 A metal washer with an opening of 8.5 0.1 mm is i to ensure that the concentrated inner core ofthe sand stream is falling in centered in the bottom opening of the funnel to restrict the S I I the center of the flow. N' 6--After 25 passes through the apparatus, resieve the sand with a No. 30 sieve to remove fines. Replace the sand after 50 passes. flow of the abrasive. 14.1.2 The disk gate installed in a slit at the top of the guide tube may be replaced by a gate in the bottom of the 10.4 Repeat 10.1 to 10.3 on at least one additional panel funnel. This gate consists of a solid metal disk attached to a coated with the material under test. long vertical screw and mounted above the washer. 14.2 Standard Abrasive8--Silicon carbide grain shall be 11. Calculation considered standard when graded as follows after a suitable 11.1 For each area of the coated panel tested, calculate the period of continuous sieving: abrasion resistance. A, in litres per mil from the following Less than 1 % retained on a No. 10 (2.00 mm) sieve equation: Maximum of 20 % retained on a No. 14 (1.40 mm) sieve A = V/T 0 % pass a No. 20 (0.85 pm) sieve where: V = volume of abrasive used, L (to one decimal place) and T = thickness of coating, mils (to one decimal place). 11.2 Calculate the mean of the abrasion resistance values obtained for different areas ofthe coated panel and the mean value of the replicate panels. 14.2.1 Use the sieves described in Specification E11. 15. Test Specimens 15.1 Prepare the coated panels as outlined in 7.1 and 7.2. ' 16. Standardization t 12. Report 16.1 Standardize the abrasion tester by the procedures : 12.1 Report the following information for each coated panel tested: ' Supporting data are available from ASTM Headquarters. Request RRIXM- i 12.1.1 Temperature and humidity during curing and at the time of testing, 1037. ,> 8 An acceptable silicon carbide grain is #16 grade Carborundum, obtains^ from the Carborundum Co., P.O. Box 423, Electro Minerals Div,, Niagara BE 12.1.2 Type and source of abrasive. NY 14302. A suitable equivalent may be used. DUP050297303 D 968 tested, tea tested, rea tested, atsd Panel jf the repli^. f of test four types of the within. to be 9 % wi^ ratories coefjj iom. Based on Id be used f0r % confidence : mean ofthree be considered sir 3316311 vaiyg i the mean of nt laboratories by more than jved substantially ion resistance ate >n, all laboratories DETEST vith two excep. 8.5 0.1 mm is l to restrict the the top of the : bottom of the k attached to a asher. grain shall be ifter a suitable n jn 8.1 and 8.2, with the following exceptions: Sjjj i.i Use silicon carbide where sand is specified. 16.1-2 Weigh the volume of silicon carbide to be intro, into the tester. Determine the efflux time for this volume. The rate of flow shall be 10 1 g/s. Conditioning (7,1 Unless otherwise agreed upon between purchaser . wi]er, condition the coated panels for at least 24 h at 23 *2*0 and 50 5 % relative humidity. Conduct the test in the environment or immediately on removal therefrom. jg. procedure jgj Measure the thickness of the coating by the proce dures *** 10.1. (8.2 Abrade the coated panel by the procedures given in 02 and 10.3 using silicon carbide as die abrasive. Deter ge the volume or weight, or both, ofabrasive used to reach <he end point. |8.3 Repeat 18.1 and 18.2 on at least one additional coated panel of the material under test. - jg. Calculation 19.1 For each area of the coated panel tested, calculate the jlflasion resistance in litres per mil from the equation given jo 10.1 or, calculate the abrasion resistance. A, in kilograms per mil from die equation: A = W/T where: W = weight of abrasive used, kg (to one decimal place) and f - thickness of coating, mils (to one decimal place). 19.2 Calculate the mean of the abrasion resistance values obtained at different locations on the test specimen and the mean values of the replicate panels. 20. Report 20.1 Report the information specified in Section 12. Abrasion resistance may be reported as litres per mil or as kilograms per mil. 21. Precision7 21.1 On the basis of an interlaboratory test of this test method in which operators in three laboratories tested four coatings having a broad range of abrasion resistance, the within-laboratory coefficient of variation was found to be 19 % with 16 degrees of freedom and the between-laboratories coefficient of variation 45 % with 8 degrees of freedom. Based upon these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 21.1.1 Repeatability--Two results, each the mean ofthree runs, obtained by the same operator should be considered suspect if they differ by more than 56 % oftheir mean value. 21.1.2 Reproducibility--Two results, each the mean of three runs, obtained by operators in different laboratories should be considered suspect if they differ by more than 147 % of their mean value. N' 8--The reproducibility of this test is improved substantially when rankings of the coatings by magnitude of abrasion resistance are used. In the interlaboratory test for evaluating precision, all laboratories ranked the coatings in the same order. 22. Keywords 22.1 abrasion (of paints/related coatings); falling abrasive tester; falling sand abrasion test; falling silicon carbide abrasion test; resistance, abrasion The American Society tor Testing and Materials takes no position respecting the validity oiany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, eitherreapproved or withdrawn. Your comments are invited eitherfor revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1516 Race St., Philadelphia, PA 19103, :ation E 11. 1 in 7.1 and 7.2. the procedures its. Request RRbOl' ,onradum. Is Div.. Niag* 121 DUP0502 97304 Designation: D 969 - 85 (Reapproved 1989)e1 Standard Test Method for Laboratory Determination of Degree of Bleeding of Traffic Paint1 This standard is issued under the fixed designation D 969; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. fi N' --Editorial changes were made throughout, including the title, in October 19S9. glass p flat po 6.2 panel i covere< tape in 6.3 . is set (a coated 1. Scope 1.1 This test method covers a laboratory test procedure for determining the degree of bleeding of traffic or pavement marking paints. 12 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D476 Specification for Titanium Dioxide Pigments2 D 867 Specification for Pumice Pigment2 D 868 Test Method for Evaluating Degree of Bleeding of Traffic Paint3 D1199 Specification for Calcium Carbonate Pigments2 2.2 Adjunct: D 868 Bleeding resistance of paint (one photo)4 3. Significance and Use 3.1 Solvents in a traffic paint may cause bleeding of pavement constituents into the traffic marking, thereby rendering the traffic marking less effective as a lane or directional indicator. This test method describes how to prepare a panel for evaluation. The very subjective method of evaluating the degree of bleeding raises Questions as to the usefulness of the result for specification compliance. 4. Apparatus 4.1 Film Applicator--A conventional type drawdown 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.44 on Traffic Coatings. Current edition approved Nov. 29, 1985. Published January 1986. Originally published as D 969 - 48 T. Last previous edition D 969 - 54 (1981)". 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTMStandards, Vol 06.01. * Copies of the pictorial photographic reference standards are contained in the publication Pictorial Standards of Coating Defects, and may be obtained from ASTM Headquarters (request Adjunct PCN 12-4086804)0) or the Federation of Societies for Coating Technology, 492 Norristown Rd,, Blue Bell, PA 19422. The original source of the photographic reference standards illustrated in Fig. 1 is the Federation. gage5 that casts a film having a minimum width of 2 in. (50 mm) and an approximate wet thickness of 15 mils (380 pm) (applicator clearance of approximately 30 mils (760 pm)). 4.2 Test Panelfor Coal-Tar Substrate--A 5 by 10-in. (127 by 254-mm) piece cut from a standard roll of so-called "15-lb (6.8-kg) coal-tar saturated asbestos or rag felt" (Note). 4.3 Test Panelfor Asphalt Substrate--A 5 by 10-in. (127 by 254-mm) piece cut from a standard roll of 15-lb (6.8-kg) asphalt-saturated felt. N' --The following paint composition, when used on 15-lb (6.8-kg) felts from various sources, gave the severe bleeding necessary for a rating of between 4 and 2 on the coal tar, and the lesser bleeding necessary for a rating between 9 and 7 on asphalt' when compared to die photographic reference standards ofTest Method D 868.4 This control paint is suggested only for use in standardizing the test panels. I Titanium dioxide TiOj/fSpecification D476, Type II, Class n> Calcium carbonate/CaCOx/ASTM Specification D 1199 Aluminum stearate (a 5% mixture in toluol shall gel below 12G*F) Pumice, No. 100 (Specification D 867) Alkyd resin solution, pure oxidizing 52 % soya oil modified, 50% solution in 38 K.B. mineral spirits V.M. & P. naphtha Lead naphthenate, 24 % Cobalt naphthenate, 6 % Chemical ASA (anti-skin agent)' Totals Pounds (kgr 219.3 525.7 2.1 87.8 425.7 53.9 5.7 1.3 1.8 1323.3 Gallons (t)* 6.25 23.29 0.23 4.48 55.98 8.78 0.59 0.16 0.24 Tooiio * 1 lb 0.454 kg. * 1 gal - 3.7854 L. 5. Preparation of Test Panel 5.1 Cut the 5 by 10-in. (125 by 255-mm) specimen panel from that portion of the roll 5 in. in from the edges. 5.2 Provide a nonbleeding contrast surface by affixing a %-in. (20-mm) cellophane tape, with firm pressure, to the entire length ofthe panel so that the outside edge of the tape is at least 1 in. (25 mm) from the edge of the panel and parallel to the edge of the panel. 6. Procedure 6.1 Place the test panel on a smooth flat surface (such as a 5 The "Bradley Blade," also known as the "Bird Film Applicator," availd* from any coating materials supply house, has been found satisfactory for l purpose. 122 DU P0502 97305 2 in. (So 380 nm) rim)), -in. (127 ;d "15-lb e). -in. (127 > (6.8-lcg) lb(6.8-kg) framing cessary for the photorol paint is lallons <L) 6.25 23.29 0.23 4.48 35.98 8.78 0.59 0.16 0.24 0.00 D 969 glass panel), with the tape side up on the left, and hold in a jjat position by weighting down the edges. 6.2 Draw the paint under test down over the specimen panel in such a manner that the entire width of the tape is Covered, leaving the remainder of the film to the right of the ^pe in direct contact with the test panels. 6.3 Keep the coated panel in a flat position until the film j5 set (after which the weights may be removed) and allow the coated panel to dry for 48 h at 70 to 80F (21 to 27C). 6.4 Immediately after completion of 48-h drying, observe the contrast in color between the portion ofthe film over the tape and that portion that is in direct contact with the test panels. Rate the degree of bleeding numerically in accord ance with the nearest photographic reference standard in Test Method D 868.4 7. Precision and Bias 7.1 Precision and bias cannot be determined. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination ol the validity of any such potent rights, and the risk of infringement ofsuch rights, are entirely their own responsibility. This standard Is subject to revision atany time by the responsible technical committee endmust be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are Invitedeitherforrevision ofthis standard ortor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a talr hearing you should make your vlaws known to the ASTM Committee on Standards, 191S Race St, Philadelphia, PA 19103. i. % i panel bring a to the letape el and *asa ivailaWe for tbit Ik k 123 DUP050297306 Designation: D 1005 - 84 (Reapproved 1990)'1 Standard Test Method for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers1 This standard is issued under the fixed designation D 1005; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This standard has been approved for me by agencies of the Department of Defense. Consult the DoD Index ofSpecifications and Standards for the specifk year of issue which'has been adopted by the Department ofDefense. Mi the are to ren spe the free 5 Me {1 N' --Figure 1 which was inadvertently deleted was editorially included in May 1990. | 6. I I 6' - 1 ti 1. Scope measurement of films on laboratory test panels. dal 1.1 This test method covers the measurement of film 3.2 The accuracy and precision of the thickness measure no thickness ofdried films ofpaint, varnish, lacquer, and related products using micrometers. Procedures A and B utilize stationary micrometers and Procedures C and D, hand-held micrometers. Procedures A and C are not recommended for films less than 0.5 mils (12.5 pm) in thickness. The min imum thickness required for Procedures B and D is a function of that required to enable removal of the sample as a free film. 1.2 The procedures appear as follows: 1.2.1 Procedure A--Stationary micrometer for measuring coatings applied to plane rigid surfaces. 1.2.2 Procedure B--Stationary micrometer for measuring free films. 1.2.3 Procedure C--Hand-held micrometer for measuring coatings applied to plane rigid surfaces. 1.2.4 Procedure D--Hand-held micrometer for measuring free films. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards; D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D2370 Test Method for Tensile Properties of Organic Coatings2 3. Significance and Use 3.1 This test method is particularly applicable to the measurement of free films and is also satisfactory for the ments may be influenced by the deformability of the coating. thici This test method is not applicable to coatings that are readily I 6. deformable under the load of the measuring instrument. with 3.3 The accuracy and precision of the thickness measure mati ments are also influenced by the uniformity of the substrate 6. ' when the coatings are applied to laboratory test panels. the'; meai 4. Apparatus 4.1 Procedures A and B: 4.1.1 The apparatus shall consist of a dial comparator, dial indicator, or micrometer. A rigid base is required for mounting the dial comparator or dial indicator gages. The presser foot of the micrometer or dial indicator shall be circular, from Vi6 to Vs in. (1.5 to 3.0 mm) in diameter, and shall be flat on the bottom. The presser foot shall be fixed to an indicator that reads to 0.1 mil (2.5 pm). The load on the Ipresser foot shall be between 20 and 40 psi (140 and 275 kPa). For Procedure B, a smooth uncoated test plate is also required. 1 4.1.2 Verify the accuracy of instrument calibration by I setting to zero with the anvils closed followed by measuring I shims of known thicknesses or standards specifically de- I signed for this purpose. Record the standard thickness gage I measurement and the micrometer reading. Use these results E to construct a calibration curve. E 4.2 Procedures C and D--The apparatus shall consist of a 1 hand-held micrometer. The anvils of the micrometer shall be i circular, from Vis to Vn in. (1.5 to 3.0 mm) in diameter, with E flat bottoms. Verify the accuracy of instrument calibration i by setting to zero with the anvils closed followed by 1 measuring shims of known thicknesses or standards specifi- 1 cally designed for this purpose. Record the standard thick- I ness gage measurement and the micrometer reading. Use M these results to construct a calibration curve. * film, slowl take 6.1 there r 0.1 xr 6.1 measi . coatir ^ has ct 6.1. the pi 1 tions propo 6.2 6.2. suitab there \ film th ^ tory w 6.2.2 the ga: reading 6.2.3 on the taken. < and tab 6.2.4 of the f v- 5. Test Specimens E 6.2.5 1 This rest method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.23 on Physical Properties of Applied Paint Films. Current edition approved Aug. 31, 1984. Published December 1984. Originally published 1949. Last previous edition D 1005 - 51(1979). 2 Annual Book ofASTM Standards, Vol 06.01. 5.1 Procedures A and C--Apply test films to a suitable plane, rigid base material from which the dried film may be satisfactorily removed. The panels shall be of sufficient size 1 to permit film thickness measurements to be made 1 in. (25 Jj mm) from any edge. 2 5.1.1 Coatings should be applied in accordance with Test j| three de 6.3 / 6.3.1 that the . Separate that oft 6.3.2 124 Jk DUP050297307 teasurecoating. ; readily tent. neasure.ubstrate els. lparator, aired for iges. The shall be eter, and i fixed to id on the and 275 ite is also ration by neasuring cally deaess gage se results nsist of a r shall be eter, with lalibration llowed by :ds specifi* lard thickiding- Use suitable .m may b fficient size de 1 in. 0 :e with Test 01005 Methods D 823 or as agreed upon between the purchaser and the seller. 5.2 Procedures B and D--Free films of the test material are required. Alternatively, the test materials can be applied to an appropriate substrate in order that they can be removed as free films without deformation. If the method of specimen preparation affects the film forming properties of the test material or requires cutting or scraping to remove the ftee film, use Procedures A or C instead. 5.2.1 Free films may be prepared in accordance with Test Method D 2370. 6. Procedure 6.1 Procedure A: 6.1.1 Mount the test panel rigidly on a suitable base. Clamp or hold it to the base in such a way that there will be no movement or spring of the panel during the film thickness measurement. 6.1.2 Close the gage slowly until contact is made, but without visible distortion of the film. Read the gage, esti mating to 0.1 mil (2.5 pm), and record the reading. 6.1.3 Open the gage and remove the film carefiilly from the area where the measurement was taken. Any suitable means, chemical or mechanical, may be used to remove the film, taking care not to distort the panel. Close the gage, slowly on the area from which the film was removed, and take a reading, estimating to 0.1 mil (2.5 pm). 6.1.4 The difference in the gage readings before and after the removal ofthe film is the thickness ofthe film. Record to 0.1 mil (2.5 pm). 6.1.5 As an alternative to the above, the panels may be measured in distinct locations prior to the application of the coating, and again in the identical locations after the coating has cured. The difference represents the coating thickness. 6.1.6 Take a sufficient number of readings to characterize the panel. A recommended minimum is three determina tions for a 3 by 6-in. (75 by 150-mm) panel and more in proportion to size. 6.2 Procedure B: 6.2.1 Mount a smooth uncoated test panel rigidly on a suitable base. Clamp or hold it to the base in such a way that there will be no movement or spring of the panel during the film thickness measurement Figure 1 illustrates one satisfac tory way of rigidly mounting the panel for measurement. 6.2.2 Close the gage slowly until contact is made. Read the gage, estimating to 0.1 mil (2.5 pm), and record the reading. 6.2.3 Open the gage and lay a free film of the test material on the panel in the same area where the measurement was taken. Close the gage slowly with care not to distort the film and take a reading, estimating to 0.1 mil (2.5 pm). 6.2.4 The difference in the gage readings is the thickness ofthe film. Record to 0.1 mil (2.5 pm). 6.2.5 When conditions permit, perform a minimum of three determinations adjacent to one another on each film. 6.3 Procedure C: 6.3.1 Hold the hand-held micrometer in such a manner 4at the micrometer can be steadied against a film surface. Separate the micrometer anvils to a distance at least twice that of the film thickness to be measured. 6.3.2 Place the coated base material between anvil con- FIG. 1 tacts. Be sure to align the panel so that it is perpendicular to the contact points. Carefully bring the micrometer anvil into contact with the film by releasing the spring tension or rotating the adjustment barrel. Do not compress the film. 6.3.3 Record the film thickness to 0.1 mil (2.5 pm). For spring-loaded micrometers, record the value directly from the dial indicator. For barrel micrometers, record the value using the instrument in the friction mode. The friction mode allows the thimble sleeve to slip without further turning the measuring screw. The friction mode provides for a consistent measuring pressure from panel to panel. 6.3.4 Open the gage and remove the film carefully from the area where the measurement was taken. Any suitable means, chemical or mechanical, may be used to remove the film, taking care not to distort the panel. Close the gage, slowly on the area from which the film was removed, and take a reading, estimating to 0.1 mil (2.5 pm). 6.3.5 The difference in the gage readings before and after the removal ofthe film is the thickness ofthe film. Record to 0.1 mil (2.5 pm). 6.3.6 As an alternative to the procedures in 6.3.2 through 6.3.5, the panels may be measured in distinct locations prior to the application of the coating, and again in the identical locations after the coating has cured. The difference repre sents the coating thickness. 6.3.7 Take a sufficient number of readings to characterize the panel. A recommended minimum is three determina tions for a 3 by 6-in. (75 by 150-mm) panel and more in proportion to size. 6.4 Procedure D: 6.4.1 Hold the hand-held micrometer in such a manner that the micrometer can be steadied against a film surface. Separate the micrometer anvils to a distance at least twice that of the film thickness to be measured. 6.4.2 Place the free film to be measured between anvil contacts. Be sure to align the film so that it is perpendicular to the contact points. Carefully bring the micrometer anvil into contact with the film by releasing the spring tension or rotating the adjustment barrel. Do not compress the film. 6.4.3 Record the film thickness to 0.1 mil (2.5 pm). For spring-loaded micrometers, record the value directly from 125 DUP0502 97308 # D 1005 the dial indicator. For barrel micrometers, record the value the instrument in the friction mode. The friction mode ments on each of three coated panels differing in film thickness, the between-laboratories standard deviations were allows the thimble sleeve to slip without further turning the found to be 0.09 mil at the 1-mil thickness level, 0.29 mil at measuring screw. The friction mode provides for a consistent the 4-mil thickness level, and 0.33 mil at the 8-mil thickness measuring pressure from film to film. level. Based on these standard deviations, the following 6,4.4 When conditions permit, perform a minimum of criteria should be used to judge the precision of results at the three determinations adjacent to one another on each film. 95 % confidence level: 8.1.1 Repeatability--Two measurements, each the mean 7. Report 7.1 Report the results as the mean thickness of a number of determinations, accompanied by a statement of the number of observations and the standard deviation of the determinations. of four replicates, obtained by the same operator should be considered suspect if they differ by more than 0.7 mil at the 1-mil thickness level and by more than 1.2 mils at the 4 to 8-mil thickness level. 8.1.2 Reproducibility--Two measurements, each the mean of four replicates, obtained by operators in different 8. Precision and Bias laboratories should be considered suspect if they differ by 8.1 Precision--On the basis of an interlaboratory study of Procedure C in which operators in two laboratories on two or three days made four replicate measurements on each of more than 0.3 mils at the 1-mil thickness level and by more than 1.1 mils at the 4 to 8-mil thickness level, 8.2 Bias--Bias has not been determined. three coated panels differing in film thickness, the within- laboratory standard deviations were found to be 0.17 mil at the 1-mil thickness level, 0.32 mils at the 4-mil thickness level, and 0.28 mil at the 8-mil thickness level. On the basis of the same interlaboratory study of Procedure C in which 9,'Keywords 9.1 dial comparator, dial indicator; dial indicator gage; film-dry film thickness; measurement of organic coatings; 51 operators in seven laboratories made four replicate measure micrometer s The American Society tor Testing and Materials takas no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ere entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapproved or withdrawn. Your commentsare invitedeitherforrevision ofthis standard orforadditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive cereful consideration at a meeting of the responsible technical committee, which you may attend. If. you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Baca St., Philadelphia, PA 19103. ,i ...4- 126 1. S' i.: paim 1.: ther atior agree proe Ann' 1.: atior addr the i appr appl 2. R 2. D D 2.: T 3. S 3. aid appl 3. seasi acco in-se 4. I 4. be g Relate DO!.: Ca publis V 700 R DUP050297309 in filmns Werg * mil at nckness 'lowing s at the e mean ould be il at the che4to ch the lifferent iffer by Vf more 3r gage; oatings; Designation: D 1006 - 73 (Reapproved 1086)*1 Standard Practice for Conducting Exterior Exposure Tests of Paints on Wood1 This standard is issued under the fixed designation D1006; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This practice has.been approvedfor use by agencies ofthe Department ofDefense to replace Method 6161.1 ofFederal Test Method StandardNo. 141A andfor listing in the DoD Index ofSpecifications and Standards. el N' --Editorial changes were made throughout in April 1986. I Scope 1.1 This practice deals only with the testing of house jjjrts and trim paints on new, previously unpainted wood. 12 This practice describes a test procedure that embodies ^ principles considered necessary for reliable results. Vari ations necessitated by circumstances may be introduced Jby agreement provided they do not violate these principles. One procedure embodying the principles is described in the Annex for use by those who find it convenient. 1,3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D358 Specification for Wood to Be Used As Panels in Weathering Tests of Coatings2 D1150 Single and Multi-Panel Forms for Recording Results of Exposure Tests of Paints2 2.2 U.S. Federal Standard: TT-W-571b Federal Specification for Wood-Preservative, Recommended Treating Practice3 3. Significance and Use 3.1 The procedure described in this practice is intended to aid in evaluating the performance of house and trim paints applied to new, previously unpainted wood. 3.2 Since natural environment varies with respect to season, geography, and topography, test results can vary in accordance with location and may not correlate to actual in-service performance (5.1). 4. Extent of Test Program 4.1 The extent of the exterior exposure test program must be governed by the breadth of the conclusions desired. The 1 This practice is under the jurisdiction of ASTM Committee D-1 on Pant and Related Coatings and Materials and is the direct responsibility of Subcommittee WU7 on Accelerated Testing. Current edition approved Oct. 29, 1973. Published December 1973. Originally Published as D 1006-51 T. Last previous edition D 1006 - 56 (1970). 1 Annual Book ofASTM Standards, Vol 06.01. 3 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn; NPODS. types of paints to be tested, the range in climatic conditions to be met, also the types of woods and structures on which the paints are to be used are important factors to be considered in establishing the exposure program. 5. Location of Test Stations 5.1 The climatic conditions of the test sites should be representative of those of the area in which the paints are to be used. The type and rate of failure of a paint film will vary when exposed to different combinations of climatic and atmospheric conditions. For reliable results, exposure sites should be selected that are representative geographically, climatically, and in atmospheric contaminations with those of the locality in which the paint will be used. To obtain conclusions that are valid for paints with national distribu tion requires exposure at several sites, selected to cover a wide range in climatic conditions.4 6. Exposure Positions 6.1 Panels for testing house paints and trim paints should be exposed on vertical test fences facing both south and north. In comparisons where dirt collection and mildew resistance are not pertinent, north vertical exposures may be omitted. There should be no obstructions close enough to shade test panels from the sun more than 2 h after sunrise, or 2 h before sunset. 6.2 In the case where it is desirable to expose coated panels in a sheltered area, such as under eaves, a suitable test fence with a sheltered or eave arrangement can be used (see Annex). 7. Construction of Test Fences 7.1 Test fences should be durable and rigid enough to remain upright under the action ofprevailing winds and frost throughout the. contemplated period: of testing.5 7.2 Lower edges of test panels, when mounted on test fences, should be at least 18 in. (460 mm) above ground level to avoid dampness and mud splash. Backs of painted boards or plywood should be protected against direct exposure to the weather by methods such as, (/) having panels on both 4 Suggested sites include the Great Lakes region, Florida, extreme southern Louisiana, the southwest region, and northeast region. 9 Fences, such as presented by W. A. Southard in the May 1959 issue of the Official Digest, are acceptable. 127 DUP050297310 # D 1006 0fthe fence, (2) mounting the panels on sheathing, and (3) the opposite side of the fence. V 7.3 Fences should have watertight caps to keep water from For best results there should be two controls--one known to perform well and one known to perform poorly. getting behind test panels. 11. Application of Paints 8. Sffrntinn of Woods for Test Panels 8.1 Paint need be tested only on woods on which it is likely to be used in practice. Conclusions drawn from tests mode 0n a limited variety of woods, however, should not be generalized for woods of other kinds. N' --See Specification 0 358. 8.2 Prior to use, test lumber and panels should be stored under such conditions that the moisture content of the wood will' be maintained within the normal range for exterior woodwork in the region in which the tests are made. 9. Construction of Test Panels 9.1 For house paints, unless the pattern of the siding requires some other choice, test panels should be made of one or the other of two patterns of siding, namely, % or 3A by 6-ia (13 or 20 by 150-mm) bevel siding or 1 by 6-in. (25 by 150-mm) drop siding. 9.2 Ifthe panels in the house paint test are not subdivided, one 3-ft (900-mm) length of 6-in. (150-mm) siding will be acceptable. Ifthe panels are subdivided, two 18-in. (460-mm) lengths are sufficient Exposures on wood panels should preferably be carried out on three panels to allow for variations in the wood. 9.3 For trim paints, the test panel should carry 1 by 4-in. (25 by 100-mm) pieces of trim lumber at each end. 9.4 A test panel of 1.5 fit2 (1400 cm2) or more in area, as provided in 9.2, may be subdivided into two or more test areas each not less than 10 in. (250 mm) long and 0,75 ft2 (700 cm2) in area. Each test area is for painting with a different paint. Paints placed on the test areas of one panel famish a comparison as to behavior. 9.5 When it will not interfere with the properties to be tested, all panels should be coated on the back to prevent warping. 10. Control or Comparison Paint for Extending the Compar isons 11:1 Ail tests that are to be compafed closely with one another should be placed on exposure as nearly simulta neously as possible. When a group of tests is too extensive for completion within a month, use a control paint or duplicate of at least 5 % ofthe test areas at successive exposure periods. 11.2 It is best in theory and practice to do the painting out-of-doors in proper weather for painting; however, indoor painting is permissible provided no more than 1 week6 elapses between successive coats and between applying the last coat and exposing on the test fence; and provided, further, that all painting is done under essentially the same drying conditions. It is necessary to allow each coat to cure sufficiently before top coating. 11.3 Preferred procedure is to apply paints with the test panel in a vertical position and kept vertical until the paint has set. If paint is spread on horizontal panels, the panels should be placed vertically immediately thereafter. 11.4 Records should be kept of the spreading rates at which paints are applied. When the purpose of the tests is to compare commercial paints, it may be appropriate to let the painter apply them at what seems to be their natural spreading rates. When the purpose is to study variation in paint composition, application should usually be at suitable predetermined spreading rates which can be controlled by applying a given weight or volume of coating to a measured area. 12. Inspections and Records 12.1 After panels have been exposed to the weather, inspections should be made after not more than 1 month, at 3 months, and at intervals of 3 months during the first 2 years, and every 6 months thereafter. Midwinter inspections, however, may be omitted in northern latitudes.7 8Inspections may be made more frequently if desired. Usually the exposures should be continued for a considerable length of time after deterioration has reached the point at which best practice calls for repainting. 12.2 Records should be kept on forms such as Standard D 1150. ,, i! ! 10.1 When several paints are to be compared, one paint 8 should be selected as a standard of comparison or "control." 6 Seventy-two hours is the preferred maximum. 7 Inspection should be made to assure that exposed panels are not covered by 'i The control paint should then be applied on one test area of accumulated snow banks. each test panel: Variations caused by wood differences are 8 These record sheets may be obtained from ASTM Headquarters (order; \ Adjunct No. 12-411500-11 and 12-411500-21) and from the Federation of revealed in the behavior ofthe control paint, and can be used Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. to adjust the ratings of the other paints to a common basis. /if 128 DUP050297311 : known t0 * wth one ly simultaitensive for r duplicatg `re periods, ie painting ver, indoor n 1 week6 ^plying the provided, y the same oat to cure ith the test il the paint the panels r. ng rates at e tests is to te to let the eir natural 'ariation in at suitable ntrolled by a measured le weather, 1 month, at the first 2 inspections, Inspections Jsually the le length of which best is Standard # D 1006 ANNEX (Mandatory Information) Al. CONSTRUCTION OF TEST FENCE AND TEST PANELS A 1.1 The plan for test fence and panels described in this Annex conforms to the principles set forth in this practice. It nresents only one of numerous possible embodiments of Jhe principles recommended. Al.2 Construction of Test Fence: Al'2.1 The test fence, or test rack, runs east and west, and . instructed to hold test panels on both sides so that there pflfwk facing both north and south. There are two rows panels, one above the other, on each side of the fence. A off cap is placed along the top of the fence, and projects approximately 1 in. (25 mm) beyond the face of the mounted panels. The fence must be sufficiently sturdy in instruction to withstand strong winds. It is mounted on wood posts that are impregnated with creosote under Pres pa in accordance with Fed. Spec. TT-W-571b. Al .2.2 Figure A1.1 shows one span or unit. The fence can be extended to as many units as the site permits or as are eeeded for the number of exposure tests to be made. ^irinnal fences may be built parallel to one another, but they should be spaced far enough apart to keep each fence jiom casting shadows on the adjacent fences during all but the first 2 h after sunrise and the last 2 h before sunset at the time of the winter solstice. Al.2.3 When cleated panels of drop siding, which do not have backing, are used, there shall always be a pair of panels, one feeing north and one facing south, to give the backs mutual protection from the weather. If for any reason there are panels on one side only of the fence, the other side shall be covered with roofing paper or other covering to protect the backs of the panels. A 1.3 Construction of Test Panels: A1.3.1 Home Paints--The boards of siding are assembled in a manner similar to house construction. Five pieces of Vi by 6-in. (13 by 150-mm) bevel siding are nailed securely on a backing of `A-in. (6-mm) plywood exterior grade, as shown in Fig: A 1.2. The top board is a blank connecting board, cut to narrower width and painted as hereinafter described. The other four boards are test boards: they may be all of one species or two each of two different species. The overlap between boards should be not less than 1 in. (25 mm). Cadmium- or zinc-coated nails, 1 Vis in. (28 mm) long, should be used and should be spaced as indicated, and clinched on the back. The lower edge of the bottom board is shimmed out from the plywood with a wood shim and the bottom board projects '/* in. beyond the shim in order to permit insertion of a panel underneath. The top of the panel, which not covered by Iquarters (order Federation of , PA 19422. FIG. A1.1 ASTM Panel Rack for Exterior Exposure of Paints 129 DUP050297312 # D 1006 is a blanlf board precoated with chalk-resisting exterior paint such as aluminum paint, is cut to a width of 4Vi in. {115 mm); the cutting makes a suitable shim for use under the bottom board. The plywood projects VS in. beyond the boards at the ends and 1 in. (25 mm) at the bottom; at the top the plywood projects 2 in. (50 mm) beyond the top ofthe second board and is overlapped by about 2lh in. (65 mm) by the top blank board. Holes are bored through the top blank board as indicated to permit positioning of the panel on the fence by means of small pegs. Holes are bored through the projecting ends of the plywood to permit secure fastening of the panels to the fence by means of wood clamps held in position by bolts with wing nuts as indicated (see also Fig. A1J). A1.3.I.I Panels made of 6-in (150-mm) drop siding jh/vilH consist of four test boards 37 in. (940 mm) long, and a narrow blank connecting board 3 in. (75 mm) wide, fitted snugly together and held by three cleats, % by 2 in. (16 by 50 mm) wide, nailed firmly on the backs. By adjusting the width of the blank connecting board the dropsiding panels can be made to lit on fences designed as shown in Fig. A 1.1, although it may be impracticable to mount both types of panel together on the same fence. Al.3.2 Trim Paints--An example of a panel for testing trim paint is shown in Fig. A 1.3. It is a modification of the panel shown in Fig. A 1.2. The modification consists in shortening the pieces of siding to 27 in. (685 mm) to make room for two pieces of trim lumber, 1 by 4 in. (25 to 100 mm), at each end; and in narrowing the exposed width ofthe siding to 4 in. to make room for another piece of trim lumber, 1 by 6 in. (25 by 150 mm), across the top. This piece is undercut, as shown in the sketch, so as to fit over the siding. The cap may be made of galvanized iron, aluminum, or painted iron. No blank connecting boards between two panels are needed. The panel may be fastened to the fence in the same way as the body paint panel. A much less elaborate panel, satisfactory in many cases, is merely a plain board, approximately 1 by 6 by 36 in. (25 by 150 by 915 mm). N' --1 in. = 25.4 mm. FIG. A1.2 ASTM Clapboard Test Panel for Exterior Exposure of Paints 130 DUP05029731 3 Is can be ig. Al.i, types of >r testing m of the nsists in to make 5 to 100 1th ofthe of trim his piece over the iminum, /een two fence in jlaborate n board, nm). D 1006 n o t ' --11n. = 25.4 mm. FIG. A1.3 ASTM Test Panel for Exterior Exposure of Trim Paints The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or ior additionalstandards andshould be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 131 DUP050297314 i Designation: D 1014 - 83 (Reapproved 1988)61 Standard Test Method for Conducting Exterior Exposure Tests of Paints on Steel1 This standard is issued under the fixed designation D 1014; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision.. A number in parentheses indicates the year of last reapprovaL A superscript epsilon (e) indicates an editorial change since the last-revision or reapproval. This lest method has been approvedfor use by agencies ofthe Department ofDefense to replace Method6160 ofFed. Test Method Std. So. 141 A andfor listing in the DoD Index ofSpecifications and Standards. 41 N' --Editorial changes were made throughout in March 1988. 1. Scope 1.1 This test method covers the determination of the relative service of exterior paints and other materials of similar purpose when applied on steel surfaces exposed out-of-doors. 1.2 Experience indicates that the steel used as a test surface has a marked bearing upon the weathering results. It is the purpose of this test method to minimize the influence of variation in steel surfaces on any series of tests by providing for uniformity in the selection of the steel surface, particularly in cooperative work. This test method also outlines uniform procedures for conducting the exposure tests and for evaluating and recording results. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address ail ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: A 36 Specification for Structural Steel12 A 283 Specification for Low and Intermediate Tensile Strength Carbon Steel Plates2 D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products3 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces3 D659 Methods of Evaluating Degree of Chalking of Exterior Paints3 D660 Test Method for Evaluating Degree of Checking of Exterior Paints3 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints3 D714 Test Method for Evaluating Degree of Blistering of Paints3 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.46 on Industrial Protective Painting. Cuirent edition approved Nov, 28, (J983, Published January 1984, Originally published as D 1014-49 T. Last previous edition D 1014-66 (1973). 2 Annual Book ofASTM Standard, Vol 01.04. 3 Annual Book ofASTM Standards, Vol 06.01. D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D1186 Test Methods for Nondestructive Measurement of Dry Film.Thickness of Nonmagnetic Coatings Applied to a Ferrous Base3 D 1212 Methods for Measurement of Wet Film Thickness of Organic Coatings3 D2200 Pictorial Surface Preparation Standards for Painting Steel Surfaces3 G7 Practice for Atmospheric Environmental Exposure Testing of Nonmetallic Materials4 3. Significance and Use . 3.1 The procedures described in this test method are intended to aid in" evaluating performance of coatings on either new or previously rusted steel. 3.2 Since the natural environment varies with respect to season and geographic location, test results may not correlate with in-service performance. 4. Base Materials for Test Specimens 4.1 A minimum of two and preferably four test specimens shall be used to evaluate the performance of any paint system. 4.2 The surface preparation for the test panels should be that, expected to be done in the field or in-service. The surface preparation shall be the same for all test panels in the test program unless, surface preparation is one of the vari ables to be evaluated. Surface preparation must be essentially identical for ail test panels, as the thoroughness of prepara tion may directly determine the performance life of the applied coating system. 4.3 The test panels should be fabricated from the same material over which the coating is expected to perform in-service. Any of the following surfaces may be used: 4.3.1 Abrasive Blasted Steel Plate--The steel plate shall conform to Specification A 36 or Specification A 283. The minimum thickness shall be `/re in. (1.6 mm). The minimum size shall be 4 by 6 in. (100 by 150 mm). Burrs and sharp projections shall be removed from the edges by filing. The test panels shall be freed of oil by suitable grease-removing solvents in accordance with Methods B, C, or D of Methods D 609. The surface shall be blasted to meet the requirements * Annual Book ofASTM Standards, Vol 14.02. 132 of Sta prepar 4.3., both,; appliec rust ar confor least 4 and 12 steel p minim project test pu grease-j or D < coating refer to from th prepara job. Nora preferabl which th. steel is i performa permittee 4.3.3 slightly, is usefril clean, u ofthe ty not less l shall be shall be; in Metht 4.4 Ai coated a: of any f surface p precautic 5. Painti 5.1 A coating method the job s 5.2 if the folkn Method Method Method Method Method Method Method DUP05029731 5 ffiiform ucts on tnent of Applied lickness rds for xposure hod are :ings on spect to correlate ecimens ly paint lould be ce. The Is in the he varisentially prepara' : of the he same perform late shall 283. The linimum nd sharp ling. The removing Methods urements D 1014 j standard D2200, Sa 2lh, if another degree of surface flfjLgtion has not been agreed upon. 0^32 Rusted Surfaces--Hot rolled steel angle or plate, or ,h. are useful for determining the performance of paints fSed to structures that cannot be thoroughly cleaned of and corrosion products. The steel angle and plate shall fflr-nn to Specification A 283. The steel angles shall be at "iW ,.... 4 ^ i/8 in. (100 by 100 by 3.2 mm) in cross section - . 12 in. (305 mm) in length. The minimum size of the piate shall be 4 by 6 in. (100 by 150 mm) with a ffrLpun thickness of '/i6 in. (1.6 mm). Burrs and sharp 'jictions shall be removed from the edges by filing. The W pieces shall be freed from oil by the use of suitable ^li.removing solvents in accordance with Methods B, C, fp 0f Methods D 609. Those persons desiring to test Ratings over rusty or slightly rusted surfaces (Note 1) should jjjlt to Standard D 2200, select the degree of rusting desired U0TB i__When testing over rusty surfaces, the test specimens should Aeferably be pre-corroded (weathered) in the same environment in Jvjj, they ultimately will be exposed. The environment in which the." ij rusted prior to painting has considerable influence on the arfotmance ofpaint applied to such steel. Artificial rusting, however, is Quitted but conditions must be stated in the test report 4.3,3 Cold-Rolled Steel Strip--Cold-rolled steel strip has a j-htiv roughened surface free from mill scale and rust, and jj useful for checking the relative performance of paints on a cjeaD) uniform surface. The steel strip shall conform to one ofthe types described in Methods D 609. The panels shall be not less than 4 by 6 in. (102 by 152 mm) in size and all edges stall be smooth and uniformly rounded. The metal panels stall be prepared by the agreed upon method (A, B, C, or D) ia Methods D 609. 4.4 After surface preparation, the panels shall be prime as soon as possible to prevent flash rusting or deposit of any foreign contaminant on the cleaned surface. After surface preparation, if the panels are stored prior to coating, precautions must be taken to preserve the clean surface. 5. Printing Test Specimens J.1 Apply all coatings in strict accordance with the coating manufacturer's written recommendations. The oethod of application expected for the production work on tie job should also be used for test panel application. 52 If the method of application is unknown select one of tie Mowing (Note 2): Method A--Automatic Spray Machine Method B--Automatic Dip Coater Method C--Manual Spray Application Method D--Motor Driven Blade Applicator Method E--Brush Application Method F--Roller Coating Method G--Curtain Coating N' 2--Details for the application of paint by Methods A, B, or D are given in Test Methods D 823. 5.3 Measure and record the film thickness of each coat in accordance with the methods recommended in Test Methods D 1186. If the test panel is covered by rust and mill scale, these methods will be less accurate, as they are influenced by the surface characteristics of this base metal. In such cases, approximations can be made by wet film thickness measure ments in accordance with Methods D 1212, or the amount of paint applied to a known area can be weighed and the average dry film thickness computed. It should be noted that even though dry film thickness measurements in accordance with Test Methods D 1186 are less accurate on surfaces with rust and mill scale than on smooth steel surfaces, they are still more accurate than those obtained by Methods D 1212 or weighing. 5.4 Allow the proper drying time between coats for multiple paint systems and before exposure as required by the coatings manufacturer and include in the test record. 5.5 Paint the back and edges ofall test specimens with the same systems as that being tested on the front of each panel. This painting provides considerable information on the behavior of the paint system on the reverse side. 5.6 The test specimens may be scribed to base metal prior to exposure. Rate any corrosion from this point ofdamage in accordance with Methods D610. 6. Exposure 6.1 The type of exposure and the position of the painted specimens may be selected from the following: 5, facing south 45, facing south 45, facing north Vertical, feeing south Vertical, facing north Insulated (backed or black box) in accordance with Practice G 7. 6.2 Mount the specimens so they do not cast shadows on each other, or contact each other or any metallic material, or any material capable of acting as a wick. Also, mount the specimens so that the products of weathering and rain water drippings do not flow from one to another. N' 3--A suitable material for the construction of racks and supports is painted wood. Metal, such as aluminum, is also suitable if the test specimens are properly insulated as by the use of porcelain or suitably selected plastic. . 7. Test Period and Rating of Paints 7.1 The test period shall be sufficient to evaluate the characteristics of the system under consideration. 7.2 Inspect at regular intervals. 7.3 Evaluate (resistance to or) degree of rusting, chalking, checking, cracking, and blistering using the following ASTM photographic reference standards: Test Methods D610, D 659, D 660, D 661, and D 714. The American Society for Testing and Materials takes noposition respecting the validity ofany patent rights ssseriedin connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ofany such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee end must be reviewed every five years and ffnot revised, either reapproved orwithdrawn. Your comments are Invited either for revision ofthis standard or toradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. fi s< ! 133 DUP050297316  n4tea 1 Designation: D 1150 - 55 (Reapproved 1987)e1 <! Standard Single- and Multi-Panel Forms for Recording Results of Exposure Tests of Paints1 This standard is issued under the fixed designation D 1 ISO; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicate:; an editorial change since the last revision or reapprovaL tl N' --Editorial changes were made throughout in May 1987. 1. Single-Panel Paint Record Form 1.1 The single-panel form2 provides on one sheet the complete exposure record of a paint test panel. It provides a record for a period of 60 months for 15 or more different types of failure. On the front side there are eight graphs upon which the record for practically every type of failure may be plotted. The type of failure is specified on six of the graphs as indicated and there are two additional graphs for special types offailure that may be required. In order to record three types of failure on a single graph the symbols X, O, and (dot) are used. The numerical system of grading is used. Ten indicates perfection or absence of failure while zero repre sents complete failure. Ratings are. plotted along the vertical axis in steps of 2. Intermediate ratings in steps of 1 may be plotted between the lines. Time is plotted along the hori zontal axis. To illustrate the use of the single-panel record form, Fig. 1 shows a section of one graph with gloss, chalking, and erosion ratings recorded. 1.2 On the reverse side of the single-panel form are columns for recording the composition, the reduction proce dure, and miscellaneous information for a paint system for as many as four coats. Ample space is provided for addi tional remarks. 2. Referenced Documents 2.1 ASTM Standards: D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces3 1 This standard is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.27 on Accelerated Testing. Current edition approved Sept. 12, 1955. Published November 1955. Originally published as D 1150 - 51 T. Last previous edition D 1150 - 55 (1982)el. 2 Copies of the single-panel form and the multi-panel inspection sheet are available from the Federation of Societies for Coatings Technology, 492 Norristown Rd,, Blue Bell, PA 19422, and from ASTM, 1916 Race St., Philadelphia, PA 19103. Request Adjunct No. 12-411500-11 (single-panel) or 12-411500-21 (multi-panel). 3 Annual Book ofASTM Standards, Vol 06.01. D659 Method of Evaluating Degree of Chalking of Exterior Paints3 D 660 .Test Method for Evaluating Degree of Checking of Exterior Paints3 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints3 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints3 D 714 Test Method for Evaluating Degree of Blistering of Paints3 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints3 2.2 Other Documents: Exposure Standards Manual4 3. Multi-Panel Paint Inspection Sheet 3.1 Although the single-panel form may be used in the field to record results directly, it is recommended that observation in the field be recorded on the multi-panel paint inspection sheet2 and later be transcribed to the single form. Provision is made on the multi-panel form for recording twenty different observations of twenty different, panels. The type of failure is to be written in the spaces under the heading "Properties." The back of the sheet may be used for remarks or any additional data that need be recorded. 4. Photographic Reference Standards 4.1 The following ASTM test methods refer to photo* graphic reference standards for use in evaluating exposure tests of paints: 4.2 Chalking--Method D 659. 4.3 Checking--Test Method D 660. 4.4 Cracking--Test Method D 661. 4.5 Erosion--Test Method D 662. 4.6 Flaking--Test Method D 772. 4.7 Rusting--Method D 610: 4.8 Blistering--Test Method D 714.' 4.9 The Exposure Standards Manual also contains picto rial standards for evaluating paint failures. 4 Available from the Federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. ttimavr. 134 DUP050297317 # D 1150 ing of dug of dng of sion of ring of taking in the d that ;1 paint 5 form, wording Is. The leading emarks photoposure FIG. 1 Sample Section of Single Panel Form Showing Gloas, Chalking, and Erosion Ratings The American Society for Testing andMaterials takes noposition respecting the validity of anypatent rights assarted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement ofsuch rights, are entirely their own responsibility. This standard Is subject to revision at any time by theresponsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments.are Invited eithertor revision ofthis standard orforadditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee an Standards, 1918 Race St., Philadelphia, PA 19103-.' s picto- ilogy, 492 135 DUP050297318 i Designation: D 1186 - 87 Standard Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base1 This standard is issued under the fixed designation D 1186; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. These test methods have been approvedfar use by agencies Ofthe Department ofDefense to replace Method 6181 of Federal Test Standard No. 141A andfor listing In the DoD Index ofSpecifications and Standards. 1. Scope 1.1 These test methods cover the nondestructive measure* ment of the dry film thickness of'nonmagnetic coatings, applied over a ferrous base material using commercially available test instruments. The test methods cover the use of instruments based on magnetic measuring principles only. Test Method A provides for the measurement of films using magnetic pull-off gages and Test Method B provides for the measurement of films using magnetic flux gages. 1.2 These test methods are not applicable to coatings that wifi be readily deformable under the load of the measuring instrument 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address ail ofthe safety problems associated with its use. It is the responsibility af the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 2.2 Steel Structures Painting Council Standard: SSPC-PA2 Measurement of Dry Paint Thickness with Magnetic Gages3 TEST METHOD A--MAGNETIC PULL-OFF GAGES 3. Summary of Test Method 3.1 Instruments complying with this test method measure thickness by using a spring calibrated to determine the force required to pull a permanent magnet from a ferrous base coated with a nonmagnetic film. The instrument must be placed directly on the coating surface to take a reading. 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.23 on Physical Properties of Applied Paint Films. Current edition approved May 29, 1987. Published July 1987. Originally published as D 1186 - 51. Last previous; edition D1186-81. 2 Annual Book ofASTM Standards, Vol 06.01. 1 Available from Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, PA 15213. .4. Significance and. Use 4.1 The attractive force of the magnet to the substrate varies inversely with the thickness of the applied film. The spring tension required to overcome the attraction of the magnet to the substrate is shown on the instrument scale as the distance (in mils or micrometres) between the magnet and the substrate. 4.2 The accuracy ofthe measurements may be influenced when made closer than 1 in. (25 mm) to an edge. 5. Apparatus 5.1 Permanent Magnet, small, either attached directly to a coil spring ("pencil" gage)4 or to a horizontal lever arm which is attached to a helical spring ("banana" gage).3 Increasing force is applied to the magnet by extending file coil spring in the first case or turning a graduated dial that coils the helical spring in the second. The readings obtained are shown directly on the instrument scale or converted by reference to a calibration curve. 6. Test Specimens 6.1 When this test method is used in the field, the specimen is the coated structure or article on which the thickness is to be evaluated. 6.2 For laboratory use, apply the materials to be tested to panels ofthe composition and surface conditions on which it is desired to determine the thickness. 1 N' 1--Applicable test panel description and surface preparation methods are given in Methods D 609. N' 2--Coatings should be applied in accordance with Test Methods D 823 or as agreed upon between the purchaser and the seller. 7. Calibration of Apparatus 7.1 Calibrate the instrument in an area free of stray magnetic fields, such as power lines, generators, or welding equipment There shall be no vibration apparent on the test piece when the instrument is being calibrated. 7.2 Use a bare section of the substrate after the specified surface preparation method has been accomplished. If an uncoated section of the substrate is not available, uncoated test panels of a similar steel type on which the specified ;, surface preparation has been performed, may be used. 4 Apparatus of the "pencil" type found to he suitable for this purpose includes Tinsley Cage, Elcometer Pencil Pun-OffCage. ` 3 Apparatus of the `banana'' type found to be suitable for tins purpose includes' Magne Cage; Mikrotest, Elcometer Inspector Thickness Gage. 136 DUP050297319 substrate 31m. The >n of the t scale as s magnet lfluenced iectlytoa ever arm " gage).5 tiding the dial that obtained verted by field, the vhich the : tested to i which it reparation with Test i the seller. of stray >r welding m the test ; specified ted. If an uncoated specified used. pose include* pose include* D 1186 Use nonmagnetic thickness shims for calibration. Id shims are non-precision and, therefore, thickness must ^verified with a micrometer. 3--Other thickness, standards such as National Bureau of Hards certified thickness calibrations standards may be used for the *-hSSw> of the magnetic pull-off gages. The use of these thickness ^Hatds requires a different calibration method as described in ^C-PA2. 74 Select calibration shims in the expected thickness ' to be measured. For example, if a coating is approxiia" w 3 mils (75 pm) in thickness, calibrate the instrument 1 mils. Then check the calibration, using shims of both a ffLer and greater thickness, to determine the thickness range ^ which the instrument will register accurately. 0 7 j Lay a calibration shim on the bare, uncoated substrate d bring the instrument magnet in direct contact with the !!Li. Remove the magnet from the shim by slowly rotating IgdSal scale ring clockwise (for helical spring-type instru ments) or lifting the entire instrument housing (for coil mring-type instruments). Hold the shim so that it will npt to during calibration, causing the magnet to lift premaujely. Observe the thickness shown on the instrument scale at the moment when the magnet breaks contact with the surface. 7.6 Ifthe instrument scale reading does not agree with the slant thickness, calibration is required. This can be accom plished by physical calibration or by drafting a calibration curve. A calibration curve involves plotting a graph with the irt,,al gage reading on one axis and the shim reading on the other. For physical calibration, consult the manufacturer's instructions. N' 4--Instruments based on the scale dial ring/helical spring can be calibrated and used in any position, while those based on the coil spring must be calibrated and used in the vertical position only. 8. Procedure 8.1 Use the instrument only after it has been calibrated in accordance with Section 7. 8.2 Assure that the coating is dry prior to use of the instrument 8.3 Inspect the magnet tip and surface to be measured to assure that they are clean. Adherent magnetic filings or other surface contaminants will affect gage readings. 8.4 Take readings in areas free of vibration, electrical, or magnetic fields. 8.5 If thickness readings are encountered outside the range of accuracy determined during calibration in 7.4, repeat the calibration procedure in that range. Check the calibration frequently during use to assure that the instru*nt continues to read properly. 8.6 Take a sufficient number of readings to characterize ike sample. 8.6.1 For laboratory measurements, a recommended minum is three for a 3 by 6-in. (75 by 150-mm) panel and oore in proportion to size. . jj-62 For field measurements, a recommended minimum B five determinations at random for every 100 ft2 (10 m2) of, !utrace area. Each of the five determinations should be the can of three separate gage readings within the area of a 'Hn. (12-mm) diameter circle. 8.7 Make measurements at least 1 in. (25 mm) away from any edge or comer of the specimen. If it is necessary to measure closer than 1 in., recheck the calibration in the specific area to determine the extent of the effect (ifany) the edge has on the measurement. 8.8 Report the instrument used, serial number, range, and mean of the thickness readings found. 9. Precision 9.1 An interlaboratory test was conducted to determine the within-laboratory and between-laboratory precision of several types of instruments in measuring a wide range of coating thickness by this method. On the basis of this interlaboratory test, the within-laboratory coefficients of variation and between-laboratory coefficients of variation were found to be those shown in Table 1 for the instruments evaluated. Based upon these coefficients of variation, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 9.1.1 Repeatability--Two results by the same operator with the same instrument should be considered suspect if they differ by more than the maximum allowable difference values shown in Table I. 9.1.2 Reproducibility--Two results, each the mean of four measurements, obtained by operators in different laborato ries should be suspect if they differ by more than the maximum allowable difference values shown in Table 1. TEST METHOD B--MAGNETIC FLUX GAGES 10. Summary of Test Method 10.1 This test method covers instruments that measure coating thickness by changes in the magnetic flux within the instrument probe or the instrument itself. The instrument probe must remain in direct contact with the coating at all times during measurement. 11. Significance and Use 11.1 The magnitude of flux changes is an inverse (nonlinear) function of the distance between the probe and the ferrous substrate. 11.2 The accuracy of the measurements may be influ enced when made closer than 1 in. (25 mm) to an edge or 3 in. (75 mm) to another mass of steel. The edge or mass of steel may cause flux leakage from the instrument, thus distorting the readings. 12. Apparatus 12.1 The testing apparatus shall be mechanically or elec trically operated. The mechanically operated instruments house an integral horseshoe magnet, the contacts of which are placed directly on the coated substrate.6 The electrically operated instruments utilize a separate instrument probe that houses the magnet and must be placed directly on the surface.7 In both types, the coating thickness is shown on the instrument scale or meter. `Apparatus of the mechanical type found to be suitable for this purpose includes Elcometer 101. 7 Apparatus ofthe probe type found to be suitable for this purpose indudes the Minitest, Minitector, Verimeter, GE Gage, Perroascope, and Accuderm. 137 DUP0502 97320 D 1186 TABLE 1 Precision of Rim Thickness Measurements Within Laboratory Coating Thickness 0.5 to 1.5 mils Test Method Instrument Degrees of Freedom (DP) Coefficient of Variation (v,,). * Maximum Allowable Difference (MAD), % Degrees of Freedom (DF) A Coll Spring Elcometer 157 12 9 12 Tinsley 12 5 12 Pooled 2? 745 22.4 4 A Helical spring Elcometer 111 12 6 12 Microtest FIM 28 5 28 MagneQage 4 & 8 Pooled 44 S3- 15.4 48 B Mechanical Elcometer 101 22 7 20.6 22 B Probe Elcometer ISO 12 5. 12 Minitest FN 250 6 5 6 GE Type 8 Gage 32 4 32 Permascopo ES 12 4 12 Verlmeter 26 3 Accuderm 4 1^ 6 Pooled 68 4.25 12.1 71 Between Laboratories Coating Thickness 0.5 to 1.5 mils Test Method Instrument Degrees of Freedom (DF) Coefficient of Variation (v*),S Maximum Allowable Difference (MAD). %. Degrees of Freedom (DF) A Coll Spring Elcometer 157 2 22 2 Tinsley 2 10 2 Pooled 1 17.1 GM 4 A Helical Spring Elcometer 111 Microtest FIM MagneQage 2 S a 5 30.5* 15- 49 a 2 8 a B Mechanical Elcometer 101 4 It 43.5 4 B Probe Elcometer 150 4 7 4 Minitest FN 250 2 GEType B 12 6 Permascope ES 6 6 5 Pooled Minitest FN 1250 22 2 6.2 18.3 22 A 12 GE Type B Verlmeter Accuderm aa a a 12 0 a * Insufficient results (or reliable estimate. 8 No interlaboratoty results provided. c Between-laboratories precision usually larger than within-laboratory precision. 5 to 17 mils Coefficient of Variation frv). * 5 4 4.53 3 2 2 2.3 3 1 2 3 2 2 2 2.4 5 to 17 mils Coefficient of Variation M.% 12 7 9.8 2 10 B 2 4 3 33.4 6 e a Maximum Allowable Difference (MAD), % 13.3 6.8 8.8 6.8 Maximum Allowable Difference (MAD), % 384. 12-2* 32.6 8 10.4 18.5 13. Test Specimens 13.1 The test specimens described in Section 6 are suit able for the instruments of Test Method B. 14. Calibration of Apparatus 14.1 Follow the steps outlined in 7.1 through 7.4. 14.2 Hold the instrument contact or probe handle firmly on the surface and perpendicular to the measuring plane during calibration and use. Follow the manufacturer's in structions for the specific adjustment of the instrument. ' N' 5--The probe-type instruments can be calibrated and used in any position, but the integral-magnet type must be recalibrated or calibration verified for each position of use. 15. Procedure 15.1 Follow the steps outlined in 8.1 through 8.7. 15.2 Take measurements no closer than 1 in. (25 mm) to an edge or 3 in. (75 mm) to another mass of steel If suck' measurements are necessary, recheck the calibration in tSe specific area to determine the effect the edge or mass of steel1' has on the instrument reading. 15.3 Report the instrument used, serial number, range, and mean of the thickness readings found. 16. Precision. 16.1 Precision--On the baas of an interlaboratory study of this test method in which several types of instruments' 138 were r diy-fij labors were s coeffic the ac 16.1 operat DUP050297321 Maximum Allowable Difference (MAD). % 133 D 1186 used in various laboratories to measure a wide range of jrv-fil thickness 011 same set of panels, the withinfboratory and between-laboratories coefficients of variation found to be as shown in Table 1. Based upon these ^efficients the following criteria should be used forjudging ^acceptability of results at the 95 % confidence level: 16,1.1 Repeatability--Two results obtained by the same jator using instruments from the same category should be considered suspect ifthey differ by more than the maximum allowable difference values given in Table 1 for the appro priate film thickness. 16.1.2 Reproducibility--Two results, each the mean of four measurements, obtained by operators in different labo ratories using instruments from the same category should be considered suspect if they differ by more than the maximum allowable difference values given in Table 1 for the appro priate film thickness. TheAmerican Society for Testing and Materials takes noposition respecting the validity of any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any tine by the.responslble technical committee and must be reviewed every five years and Ifnotrevised, either reepproved or withdrawn. Yourcomments ere Invitedeither for revision ofthis standard orlor additional standards and should be addressed to ASTM Headquarters. Your comments will receive caroful consideration at amoating of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to thaASTM Committee on Standards, 1916 Haas St., Philadelphia, PA 19109. 8.S Maximum Allowable Difference (MAD), % 38.6. 122* 32.6 8 ugh S.7. in. (25 mm) to of steel. If such Jibration in the or mass of steel number, range. laboratory studf i of instruments T'.i-! '... 139 DUP050297322 Designation: D 1200 - 88 th. Standard Test Method for Viscosity by Ford Viscosity Cup1 This standard is issued under the fixed designation D 1200; the number immediately fallowing the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This standard has been approvedfar use by agencies ofthe Department of Defense to replace Method 4282 ofFederal Test Method StandardNo. 141. Consult the DoD Index ofSpecifications and Standardsforthe specific year ofissue which has been adopted by the Department ofDefense. 1; Scope 1.1 This test method covers the determination of the viscosity of Newtonian or near-Newtonian paints, varnishes, lacquers, and related liquid materials with the Ford-type efflux viscosity cup. If the material is non-Newtonian, that is, shear-thinning or thixotropic, Test Method D2196 should be used. 1.2 This standard may involve hazardous materials, opera ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D2196 Test Methods for SJieological Properties of Non- Newtonian Materials by Rotational (Brookfield) Viscometer12 E 1 Specification for ASTM Thermometers3 3. Terminology 3.1 Definitions: 3.1.1 Newtonian liquid--a liquid in which the viscosity is independent of the shear stress or shear rate. If the ratio of shear stress to shear rate is not constant, the liquid is non-Newtonian. 3.1.2 Near-Newtonian liquid--a liquid in which the vari ation of viscosity with shear rate is small and the effect on viscosity of mechanical disturbances such as stirring is negligible. 4. Summary of Test Method 4.1 The Ford viscosity cup is filled level full with the liquid under test, and the time for the material to flow through one of the standard orifices is measured. 5. Significance and Use 5.1 This test method is useful for the determination of package and application viscosities of a number of paints pd other coatings and in the thinning ofthese materials, but is limited to Newtonian or near-Newtonian liquids. 5.2 There are other types of apparatus for measuring viscosity in the laboratory that produce more accurate results. 6. Apparatus 6.1 Ford Viscosity Cups--Nos. 1, 2, 3, 4, and 5 Ford viscosity cups made of corrosion- and solvent-resistant materials assembled as complete units (Note 1), and con forming to the dimensional requirements shown in Fig. 1. The orifice dimensions are considered as a guide only as the combination of cup and orifice dimensions must permit conformance to the flow formula for each cup as listed in the Appendix. N' 1--If the orifice is removed from the cup for any reason the cup should be recalibrated before use as described in the Appendix. 6.2 Thermometer--Saybolt Viscosity Thermometer con forming to the requirements for Thermometer 17C (19 to 27CC) or 17F (66 to 80"F) as prescribed in Specification E I. 6.3 Timing Device--Any timing device may be used providing that the readings can be taken with a discrimina tion of 0.2 s or better. 7. Test Specimen 7.1 The specimen of the material to be tested shall be visibly homogeneous and free of any foreign material or air bubbles. 8. Temperature of Testing 8.1 All measurements with the Ford viscosity cups shall; be made at 77F (25<'C) or a temperature agreed upoa| between producer and user. Temperature drift during the test* should be kept to a minimum and should not exceed 0.4F (0.2*Q. N' 2-- It is impossible to predict the effect oftemperature change| on each material with which the apparatus may he used. This factor may s be less than 1 % per degree Celsius for some liquids whereas others may 1 be as high as 8 to 10 % per degree Celsius. 10 be ai StE de en 11 dr; de; 72 at sw 9.5 n 1 This test method is under the jurisdiction ofASTM Committee D-l on Paints and Related Coatings and Materials and is the direct responsibility of Subcom mittee OOI.24 on Physical Properties of Liquid Paints and Palm Materials. Current edition approved Oct. 31, 1988. Published December 1988. Originally published as D 1200 - 52 T. Last previous edition D 1200 - 82. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Voi 14.03. 9. Calibration 9.1 Cups should be calibrated in accordance with thefl procedure described in the Appendix. The frequency of thi|i| calibration check depends upon the amount of use and the' care that the individual cup receives. If the cup varies more 140 DUP050297323 ials, but :asuring iccurate 5 Ford resistant nd coni Fig. 1. y as the permit din the eason the jndix. ter con: (19 to ion E 1. be used crimina- >hall be il or air ,,ps shall id upon g the test d 0.4T are change factor may rthers may with the ;y of this ; and the 0 1200 jjjan 10 % from standard, it should not be'used. jQ. Conditioning 10.1 Bring the material to a temperature a few degrees ^low that desired and then agitate vigorously for 10 min on a reciprocating shaker in a pint can two-thirds full. Allow to jjand undisturbed for 10 min while adjusting further to the desired temperature. Make the viscosity determination at the end of the 10-min period. jl. procedure tl.l Make viscosity determinations in a room free of drafts and rapid changes in temperature. For the highest degree of precision the room temperature should be between 72 and 82F (22 and 28C). Determinations should be made jt a temperature above the dew point of the atmosphere surrounding the apparatus. 11.2 Choose the proper cup so that the time of efflux will be between 20 and 100 s (preferably between 30 and 100 s) for cup Nos. 3, 4, and 5; between 55 and 100 s for cup No. 1; and between 40 and 100 s for cup No. 2 (Fig. 2). 11.3 Level the instrument so that a cup may be filled level full without a meniscus or overflow at one side. 11.4 Determine the time in seconds of efflux as follows: Close the orifice, for example, by holding a rubber stopper against it. Fill the cup with the prepared specimen. The preferred method is to overfill the cup and scrape off the excess with a straightedge. Pull the stopper away and simultaneously start the timing device. Measure the time until the first break in the stream. 11.5 Measure the temperature of the fluid in the efflux stream. 11.6 If the cup has been established to be nonstandard when calibrated as described in the Appendix, apply the percent difference to the measured seconds to get the corrected viscosity in Ford-cup seconds. 12. Care of Cup 12.1 Following each determination, clean the cup by the use of a suitable solvent and a soft brush. Under no conditions should metal cleaning tools be brought into contact with the instrument. Particular care must be exer cised in cleaning the orifice to avoid any film deposit or nicks on the inside walls. 13. Report 13.1 Report the following information: 13.1.1 The efflux time to the nearest 0.2 s for the cup orifice combination (for example, viscosity 33.2 s with No. 4 Ford- cup), the temperature of the test specimen (as in the efflux stream), and the immediate history of agitation and rest prior to the measurement. --12.7 mm-- -- 12.7 mm--* --j 7.6mm |-- /9.5mm--24N.F;2Thd j6n 14. Precision and Bias 14.1 On the basis of an interlaboratory test of this test method in which eight cooperators from four different laboratories made measurements on five different paints, the within-laboratory coefficient of variation was found to be 2.8 % with 35 df and the between-laboratory coefficient of l variation was found to be 6.9% with 30 df. Based on these coefficients, the following criteria should be used for judging Orifice No. 1 No. 2 No. 3 No. 4 No. 5 - A, mm 1.90 2.S3 3.40 4.12 5.20 Ford Viscosity Cup and Orifices EFFLUX TIME IN SECONDS FIG. 2 Approximate Viscosity Curves for Ford Cups 14L DUP050297324 # D 1200 the acceptability of results at the 95 % confidence level: 14.1.1 Repeatability--Two results obtained by the same operator on different days should be considered suspect if they differ by more than 8 %. 14.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than 20 %, IS. Index Terms 15.1 This test method is indexed under the following terms: flow cup; viscometers--Ford; Ford cup. APPENDIX XI. Calibration Procedure for Ford Caps XI.1 The orifice of the Ford cup is commonly made of brass or some other corrosion-resistant material which is subject to wear with use and cleaning. A small change in diameter of the orifice becomes significant in the results obtained with the use of this type of viscosity-measuring apparatus. X1.2 The viscosity standards4 are available only as 1-pt samples. XI.3 Select the appropriate liquid viscosity standard for the cup to be calibrated (see Table Xl.l). Bring this cup and the liquid viscosity standard to a constant temperature as close as possible to 77.0'F (25.0C) or to the operating temperature of the cup. Determine the time of efflux to the nearest 0.2 s using the procedure detailed in Section 11. Keep the temperature drift to within 0.4F (0.2"C). If the temperature is not 77F, the actual temperature must be noted and the viscosity of the standard oil corrected to this temperature. XI.4 The following formulas are used to convert the time of flow in seconds, t, to kinematic viscosity V: 4 Certified kinematic viscosity standards are available from the Cannon Instrument Co., P-O. Box 16, State College, Pa. 16801. For particular oils applicable for use with the Ford Cups referto Table Xl.l. Oils available from other sources, having known kinematic viscosities, may also be used. V, = 0.49 (1 - 35.0) V2 = 1.44 (t - 18.0) V3 = 2.31 (t - 6.58) V4 = 3.85 (t - 4.49) Fj = 12.1 (t - 2.00) where Vx, V2, V3, V4, and Vs = kinematic viscosity using orifice No. 1; 2, 3,4, and 5, respectively, cSt. TABLE Xl.l Viscosity Standards Recommended for Calibrating Ford Viscosity Cups Cup Number 1 2 3 4 5 Approximate Cup Viscosity Range, cSt 10 to 35 25 to 120 49 to 220 70 to 370 200 to 1200 Standard Oil Designation S-10 S-20 S-60 S-60 S-200 Approximate Designated Viscosity at 77F (25'C), cSt4 20 35 120 120 460 A Exact viscosities are supplied with the oil samples. XI.5 The difference between the certified viscosity and the determined viscosity, multiplied by 100 and divided by the certified viscosity, will give the percent variation of the cup from standard. A percent correction can be applied to the seconds flow when the cup is in normal use. If the qip varies more than 10 % from standard, it is recommended that the orifice be replaced and that the cup be recalibrated. '/ The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised'that determination of the validity ofany such patent rights, end the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnotrevised, either reapproved or withdrawn. Your comments areInvited either for revisionofthisstandardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not receded a fair hearing you should make your views known to the ASTM Committee on Standards, 7976 flees St., Philadelphia, PA 19103. 1. : 1 me (Nc coll teri coli N sent D3f 1 atic ada the app app spec 1. plie 2. I 2 E D D E E E | i and R i mittee I' Cur t Publisl 142 DUP050297325 Designation: D 1209- 84 (Reapproved I988)e1 following Standard Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)*1 This standard is issued under the fixed designation D 1209; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4243.1 ofFederal Test Method Standard No. 141. Constdt the DoD Index tfSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. " N ' --Paragraph 1.3 and Footnotes 6, 7, and 10 were added editorially and subsequent footnotes renumbered in March 1988. :osity using ' Calibrating Approximate cosity at 77T 25C). cSt* io 35 120 120 460 scosity and divided by ition of the applied to . If the cup ommended ;calibrated. 1. Scope 1.1 This test method describes a procedure for the visual measurement of the color of essentially light colored liquids (ffote 1)- It is applicable only to materials in which the color-producing bodies present have light absorption characjeristics nearly identical with those of the platinum-cohalt color standards used. N' I--A procedure for estimating color of darker liquids, de scribed for soluble nitrocellulose base solutions, is given in Methods D365. 1.2 This standard may involve hazardous materials, operotions, and equipment. This standard does not purport to address all ofthe safetyproblems associated with its use. It is the responsibility of the user of. this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements see Section 6. 1.3 For hazard information and guidance, see the sup plier's Material Safety Data Sheet. 1. Referenced Documents 2.1 ASTM Standards: DI56 Test Method for Saybolt Color of Petroleum Products (Saybolt Chromometer Method)2 D365 Test Methods for Soluble Nitrocellulose Base Solutions3 D1193 Specification for Reagent Water4 E 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals5 E 202 Method for Analysis of Ethylene Glycols and Propylene Glycols5 E 346 Method for Analysis of Methanol6 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint rad Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Current edition approved April 27, 1984. Published August 1984. Originally Published as D 1209 - 52. Last previous edition D 1209 - 79. 1 Annual Book ofASiTM Standards, Vol 05.01. 3 Annual Book ofASTM Standards, Vol 06.02. " Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 15.05. * Annual Book ofASTM Standards, Vol 15.05. 3. Significance and Use 3.1 The property of color of a solvent varies in impor tance with the application for which it is intended, the amount of color that can be tolerated being dependent on the color characteristics of the material in which it is used. The paint, varnish, and lacquer solvents, or diluents com mercially available on today's market normally have little or no color. The presence or absence of color in such material is an indication of the degree of refinement to which the solvent has been subjected or of the cleanliness of the shipping or storage container in which it is handled, or both. 3.2 For a number of years the term "water-white" was considered sufficient as a measurement of solvent color. Several expressions for defining "water-white" gradually appeared and it became evident that a more precise color standard was needed. This was accomplished in 1952 with the adoption of Test Method D 1209 using the platinumcobalt stale. This test method is similar to the description given in Standard Methods for the Examination of Water and Waste Water7 and is referred to by many as "APHA Color." The preparation of these platinum-cobalt color standards was originally described by A. Hazen in the American Chemical JoumaP in which he assigned the number 5 (parts per ten thousand) to his platinum-cobalt stock solution. Subsequently, in their first edition (1905) of Standard Methods for the Examination of Water, the American Public Health Association, using exactly the same concentration of reagents, assigned the color designation 500 (parts per million) which is the' same ratio. The parts per million nomenclature is not used since color is not referred directly to a weight relationship. It is therefore recommended that the incorrect term "Hazen Color" should not be used. Also, because it refers primarily to water, the term "APHA Color" is undesirable. The recommended nomenclature for referring to the color of organic liquids is "Platinum-Cobalt Color, Test Method D 1209." 3.3 The petroleum industry uses the Saybolt colorimeter Test Method, D 156 for measuring and defining the color of hydrocarbon solvents; however, this system of color mea surement is not commonly employed outside of the petro- 7 Standard Methods for the Examination of Water and Waste Water-, M. Franson, Ed., American Public Health Assoc., 14th ed., 1975, p. 65. 8 Hazen, A., "New Color Standard for Natural Waters," American Chemical Journal, Vol XIV, 1892, p. 300-310. 143 DUP050297326 f D 1209 TABLE 1 Absorbance Tolerance Limits For No. 500 PlatinumCobalt Stock Solution Wavelength, nm Absorbance 430 0.110 to 0.120 455 0.130 to 0.145 480 0.105 to 0.120 510 0.055 to 0.065 ieum industry. It has been reported by various sources that a Saybolt color of +25 is equivalent to 25 in the platinumcobalt system or to colors produced by masses of potassium dichromate ranging between 4.8 and 5.6 mg dissolved in 1 L of distilled water. Because of the differences in the spectral characteristics of the several color systems being compared and the subjective manner in which the measurements are made, exact equivalencies are difficult to obtain. 4. Apparatus 4.1 Spectrophotometer, equipped for liquid samples and for measurements in the visible region.9 N' 2--The spectrophotometer used must be clean and in fust- class operating condition. The instrument should be calibrated in accordance with the instructions given in the Standards for Checking the Calibration of Spectrophotometers (200 to 1000 nm).10 4.2 Spectrophotometer Cells, matched having a 10-mm light path. 4.3 Color Comparison Tubes--Matched 100-mL, tailform Nessler tubes, provided with ground-on, optically clear, glass caps. Tubes should be selected so that die height of the 100-mL graduation mark is 275 to 295 mm above the bottom of the tube. 4.4 Color Comparator--A color comparator constructed to permit visual comparison of light transmitted through tail-form, 100-mL Nessler tubes in the direction of their longitudinal axes. The comparator should be constructed so that white light is passed through or reflected off a white glass plate and directed with equal intensity through the tubes, and should be shielded so that no light enters the tubes from the side.11 5. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.12 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water TABLE 2 Platinum-Cobalt Color Standards Color Standard Number Stock Solution, mL Color Standard Number Stock Solution, mL 5- 1 70 14 10 2 100 20 15 3 150 30 20 4 200 40 25 - 5 250 50 30 6 300 60 35 7 350 70 40 8 400 80 50 10 450 90 60 12 500 100* 'This is platinum-cobait color No. 10 In Methods D 365. conforming to Type IV of Specification D 1193. 5.3 Cobalt Chloride {CoG2`b1i20). 5.4 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 5.5 Potassium Chloroplatinate (K2PtCl6). i TABL c r most color i of the 9.2 and tl report and re 6. Hazards 6.1 Concentrated hydrochloric add is a corrosive chem ical. 7. Platinum-Cobalt Reference Standards 7.1 Platinum-Cobalt Stock Solution--Dissolve 1.245 g of potassium chloroplatinate (K2PtCl<;) and 1.00 g of cobalt chloride (CoCl2 6H20) in water. Carefully add 100 mL of hydrochloric add (HO, sp gr 1.19) and dilute to 1 L with ; water. The absorbance of the 500 platinum-cobalt stock 1 solution in a cell having a 10-mm light path, with reagent water in a matched cell as the reference solution,13 must fell [ within the limits given in Table 1. { 7.2 Platinum-Cobalt Standards--From the stock sohi- | tion, prepare color standards in accordance with Table 2 by ? diluting the required volumes to TOO mL with water in the l Nessler tubes. Cap the tubes and seal the caps with shellac or a waterproofcement. When properly sealed and stored, these standards are stable for at least 1 year and do not degrade markedly for 2 years.14 7.2.1 For a more precise measurement of light colon below 15 platinum-cobalt, prepare color standards from the stock solution in accordance with Table 3 by diluting the 1 required volumes to 100 mL with water in the Nessler tubes, 1 Use a semi-microburet for measuring the required amount of 1 stock solution. ' K 10. Pr 10.1 10.1. interlal ards h. prepare 7 of tb solutioi laborati then rei were ret for solu units fo to the r 13 Supr DO 1-1024 8. Procedure 1 8.1 Introduce 100 mL of specimen into a Nessler tube, i passing the specimen through a filter if it has any visible : turbidity. Cap the tube, place in the comparator, and ; compare with the standards. 'The Beckman Model B and its equivalents have been found satisfactory for this purpose. 10 See National Bureau of Standards Letter Circular LC-I017. :J '1 A unit available from Scientific Glass and Instruments, Inc., P.O. Box 6, Houston, TX 77001, has been found suitable for this purpose. 11 "Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc.. New York, NY, and the "United States Pharmacopeia." 9v Report 9.1 Report as the color the number of the standard that 13 See the manufacturer's instruction manual for complete details for opentsl the spectrophotometer. 14 Scharf, W. W,, Ferber, R. H,, and White, R. G,, "Stability of PlatanCobalt Color Standards," Materials Research arid Standards, Vol 6, No. 6. A* 1966, pp. 302-304. 144 DUP050297327 D 1209 rated hydro- rosive chem- ve 1.245 g of t g of cobalt d 100 mL of to 1 L with -cobalt stock with reagent n,13 must fall stock soluth Table 2 by water in die /ith shellac or 1 stored, these > not degrade light colors rds from the diluting the lessler tubes. :d amount of TABLE 3 Platinum-Cobalt Color Standards for Very Light Colors Color Standard Number Stock Solution, mL Color Standard Number Stock Solution, mL 1 0.20 9 1.80 2 0.40 10 2.00 3 0.60 11 2.20 4 0.80 12 2.40 5 1.00 13 2.80 6 1.20 14 2.80 7 1.40 15 3.00 8 1.60 most nearly matches the specimen. In the event that the color lies midway between two standards, report the darker 0f the two. 9.2 If, owing to differences in hue between the specimen and the standards, a definite match cannot be obtained, (eport the range over which an apparent match is obtained, and report the material as "ofF-hue." 10. Precision15 10.1 Color Standards: 10.1.1 These precision statements are based upon an interlaboratory study in which five platinum-cobalt stand ards having values of 25, 75, 170, 385, and 475 were prepared in accordance with the instructions given in Section 7 of this test method and were given coded labels. These solutions were tested by one analyst in each of ten different laboratories making a single observation on one day and then repeating the observation on a second day. The analysts were requested to estimate the color to the nearest one unit for solutions below 40 platinum-cobalt, to the nearest five units for solutions between 40 and 100 platinum-cobalt and to the nearest ten units for solutions above 100 platinum- cobalt. In this interlaboratory study, the within-Iaboratory coefficient of variation was found to be 1.8 % with 60 degrees of freedom, and the between-laboratories coefficient of variation was found to be 5.3 % with 54 degrees of freedom. Based on these results, the following criteria, calculated in accordance with Practice E 180, should be used forjudging the acceptability of results at the 95 % confidence level when the results are obtained under optimum condi tions where the hue of the sample matches exactly the hue of the standards. Poorer precision will be obtained in varying degrees as the hue of the sample departs from that of the standards. 10.1.1.1 Repeatability--Two results, obtained by the same analyst on different days, should be considered suspect if they differ by more than 5.1 %. 10.1.1.2 Reproducibility--Two results, obtained by ana lysts in different laboratories, should be considered suspect if they difFer by more than 15 %. 10.2 Specimen:16 10.2.1 In an interlaboratory study of this test method in which the standards described in Table 3 were used, the within-Iaboratory standard deviation was found to be one platinum-cobalt unit at 56 degrees of freedom and the between-laboratory standard deviation was found to be 2 platinum-cobalt units' at 25 degrees of freedom. Based on these standard deviations, the following criteria should be used for judging, at the 95 % confidence level, the accept ability of results obtained on light colored samples. 10.2.1.1 Repeatability--Two results, each the mean of duplicates, obtained by the same operator on different days should be considered suspect if they difFer by more than two platinum-cobalt units. 10.2.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than seven platinum-cobalt units. lsSupponing data are available from ASTM' Headquarters. Request RR; D01-IQ24. 16 These precision statements are based on interlaboratory studies conducted by Committee E-IS on Industrial Chemicals on samples of ethylene glycol and methanol as reported in Method E 202, Method E 346, and research report RR: E15-28. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard! Users at this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such.rights, ere entirely their own responsibility. Nessler tube, as any visible iparator. and This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not revised, eitherreapproved or withdrawn. Yourcomments are invited eitherfor revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. standard that itjnuro- 6, A"* 145 DUP050297328 1 Designation: D 1210 - 79 (JReapproved 1988)1 Standard Test Method for Fineness of Dispersion of Pigment-Vehicle Systems1 This standard is issued under the fixed designation D 1210; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval, A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 41 N' --Editorial changes were made throughout in June 1988. 1. Scope 1.1 This test method covers measurement ofthe degree of dispersion (commonly referred to as "fineness of grind") of the pigment in a pigment-vehicle system such as liquid coatings and their intermediates. It may also be used to assess the inclusion of particulates by a cleanliness rating. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish, appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Summary of Test Method 2.1 The product is spread by means of a scraper in a calibrated tapered path. At some point in this path, particles or agglomerates, or both, will become visible. A direct reading from the calibrated scale is then made at the point where the particles form a definite pattern. When the single path gage is used it is also possible to rate "cleanliness" (see 6.2). 3. Significance and Use 3.1 In making pigmented products, the pigment is usually dispersed in a portion of the vehicle in some sort of mill. At this stage, it is necessary to be able to judge if the pigment agglomerates have been sufficiently broken up so as not to interfere with the smoothness of the finished coating film. This test method describes a way of making this judgment 4. Apparatus 4.1 Gage--A hardened steel, stainless steel, or chrome- plated steel block (Fig. 1) approximately 6.7 in. (170 mm) in length, and 0.6 in. (15 mm) in thickness. The top surface of. the block shall be ground smooth and planar and shall contain one or two paths 5 in. (127 mm) in calibrated length. The path shall be tapered uniformly in depth lengthwise from 100 pm (about 4 mils) at 10 mm from one end to zero depth at the other with intermediate calibrations in accord ance with the depth at those points. Preferred calibrations are 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials; and is the direct responsibility of Subcom mittee DO 1.24 on Physical Properties of Liquid Paint and Paint Materials. Current edition approved Nov. 30, 1979. Published January 1980. Originally published as D 1210 - 52. Last previous edition D 1210 - 78. Hegman units and micrometres (Note 1). Two path widths are covered by this test method: 4.1.1 Two parallel paths each 0.5 in. wide (12.5 mm) and spaced 0.5 in. apart centered in a block 2.5 in. (65 mm) wide. 4.1.2 One path 2 in. (50 mm) in width centered in a block 3.5 in. (90 mm) wide. N' t--Several arbitrary scales and modifications of the gage are used by industry. In order that readings obtained with these arbitrary scales and modifications can be reported in the preferred units, the approximate relationship of these scales to gage depth is shown in the following example: Hegman Scale-4 Depth, pmfl Depth, mils* PC or FSPT Seale c NPIRI Sc41e 0 1 2 3 4 5 6 7 8 1 100- 90 75 65 50 40 25 . 15 0 4 . 3.5 3 2.5 2 1.5I 0.5 0 0 l'/ 2'A 3V 5 m V/i 8% 10 40 35 30 25 20 15 10 5 0 A Sometimes referred to in error as the North Standard scale. B Rounded to nearest 5 gm or 0.5 mil. c Federation of Societies for Paint Technology scale. National Printing Ink Research Institute scale, 0 to 10 on the NPIRJProduction Grindometer, but extended on many gages to 20 or 30. 4.2 Scraper--A double-edged hardened steel, stainless steel, or chrome-plated steel blade (Fig. 2) 3.75 in. (95 nun)' long, 1.5 in. (38 mm) wide, and 0.25 in. (6.4 mm) thick. Tfit two edges on the 3.75-in. sides shall be rounded to a radius of 0.015 in. (0.38 mm). 5. Care of Gage 5.1 Clean the gage immediately after each use. Use solvent and a soft cloth. Keep the gage covered or encased all times when not in use. Protect gages that lie idle f extended periods of time from rust with an oil coating or soaked wrap. 5.2 Do not allow any hard materials to come in with the gage surface or scraper in any manner that result in scarring or nicking. Avoid tapping or serai with other metal. 5.3 The scraper may be rendered unsatisfactory for use wear or nicks of the contact edge or warpage (Note Replace or recondition unsatisfactory blades. N' 2--Wear or warpage of the scraper may be noted by faring edge of the scraper down on the smooth level face of the gage, tnspec gage. ! to wet face si use. 146 DUP050297329 D1210 / H 0- / -100 1_ -so 2- 3- -60 th widths mm) and am) wide, in a block he gags are se arbitrary 1 units, the iown in the NPtRI Scale0 40 35 30 25 20 15 10 5 0 A- -- -40 5- 6-20 7- -- -A s>- i Two-Path Gage ) HMtwvttne the contact edge by means ofa strong light, placed behind the , the NPIRl forward or back will reveal poor contartdue wwge. Any light coming through between scraperand gage stainless (95 mm) &ce shows thatthe scraper has been damaged and is not satisfactory for 1 ose. hick. The radius of 6.Visual Standards 6.1 The diagrams in Fig. 3 are reproductions of ax typtcsd I fineness gage patterns with the double-path gage in 4.1.1, and they should be viewed with the purpose of standardrang the se. Use a enfcased at ie idle for iting or oil relationship of particle distribution to fineness desolation The arrow?n each drawing represents the end point (readmg) for that distribution. These patterns are to be usedfor notation of frequency of particles and shouldnot be mtermeted according to the size of the dots. Although called in contact that might "standards" they are really examples qf fineness readings to he used as a guide, since no two particle distnbutipns will be scratching ^^Simikrtyt'Fig. 4 exhibits typical fineness gage patterns for use by (Note 2). I for the 2-in. (Sl-mm) gage in 4.1.2. These diagrams are to be used like those for the double-path gage except that a "cleanliness" rating is also shown. "Qeapliness is descrip tive ofthe number of particles that appear in the pafo above the fineness designation. Three ratings are indicated. A (0 to 8 specks), B (9 to 15 specks), and C (16 or more specks). by facing the e gage, then 147 DUP050297330 # D 1210 H H ^Qrn o- -IOO 1- 2- 0 -75 m 0 W t 0 # *- 4 - <" * * -50 *.* 0 ***' /. . - * * X 5- ;* !viV 6- ** * k. #,.v * '* -- -25 7- >*.* ` *,, . 3 --. . . r. - i 8- -0 1V Hegman BO pm 3V4 Hegman FIG. 3a Typical Fineness Gage Patterns 60 pm 7. Procedure slightly. When using the double-path gage, place material in 7. i Place the gage on a horizontal fiat, nonslippery surface and wipe clean immediately before the test. Be sure the gage surface is free of lint. 7.2 Hand stir the specimen (Note 3) vigorously for 2 min, taking care that air bubbles are not whipped into the paint. To be sure of an accurate grind reading, specimens must be free of air bubbles. N ' 3--For this test method to function properly, the pigment particles in the specimens to be tested should be free to settle to the bottom of the gage channel after the drawdown. Therefore, before testing, high-viscosity intermediate specimens that have little ability to flow should be reduced with a compatible liquid. Reduction should be in approximately the same proportion as the intermediate will be reduced both paths. 7.4 Holding the scraper in both hands, nearly vertical but inclined slightly toward the operator, draw the material \ down the length of the path toward the shallow end of t$ gage with a uniform, brisk motion in approximately 1 to 2 s, Exert upon the scraper only sufficient pressure to deal excess material from the face of the gage. Within 10 s f placing the specimen on the gag?, make a reading as follows. 7.4.1 View the gage from the side, perpendicular to the length of the path. Keeping the gage between the opera# and the light source, make the angle between the face of the gage and the line of vision between 20 and 30. 7.4.2 definite and 4).' gage, av Hegmac 7.5 A prelimin eating t Procedui readings made w drawdou reported 1 'i in practice. 7.3 Immediately place the material to be tested in the deep end of the path, or paths, so that it overflows the path N' 4--Gear finishes may have to be viewed at a lower angled1 they may have to be opacified with a finely ground colorant or dye i* | order to see better the particles of flatting pigment. the two) 7-6 In 7.6.1 : 148 DU PO50297331 T H 01210 H material in vertical but he material end of the :ely 1 to 2 s. re to clean hin 10 s of g as follows: cular to the :he operator e face of the lower angle or jrant or dye18 4 Hegman 50 (im 4V Hegman FIG. 3b Typical Flnenea* Qaga Patterns 40 nm 7.4.2 Observe the point where the material first shows a definite speckled pattern, not just isolated specks (see Figs. 3 ffld 4). This is the fineness reading. When using the two-path Pge, average the values id the two paths to the nearest JA Htgman unit. This average is considered one reading. 7.5 After the first drawdown and reading, which are Preliminary for establishing proper test conditions and loBting die position of the fineness reading, repeat the Procedure twice, beginning with 7.3, to obtain two test ^ngs. This process allows the two test readings to be ade with limited time lapses between completion of "Gwdown and reading. (Do not consider any reading for the "ported fineness when die time lapse exceeds 10 s.) Average w two readings to the nearest V* Hegman units (5 jim). '6 Interpretation ofDispersion Pattern: '6.1 Inspect the initial drawdown for pattern, and the- approximate fineness. Determine the point in the particle distribution that approximates a similar end point pattern to that of the pictorial standards. 7.6.2 Judge cleanliness on the one-path gage either by comparison to the typical fineness patterns (shown only at a 6 Hegman level but applicable, by analogy to any fineness level) or by coiinting nibs coarser than the selected fineness level (see 6.2 for cleanliness ranges). 8i Report ' 8.1 Report' the following information: 8.1:1' whether die two-path gage in 4,1.1 or the one-path gage in 4.1.2 was used. 8.1.2 The average of two readings conforming to the conditions of 7.6. Report micrometre readings to the nearest 149s DUP050297332 Dr 1210 i; ;|ii multiple of 5 pm and Hegman readings to the nearest'Aunit. these standard deviations and the requirement that readings 8.1.3 Cleanliness may be reported also when using the are..tp be reported to the nearest.'A Hegman unit or multiple | two-path gage. of fTpm, the Mowing criteria should be used for judging the | 9. Precision and Bias2 preosiqn of results at a 95'% confidence level: . y\ 9.1.1"Repeatability--Two results, obtained by a single 9.1 On the basis of an interlaboratory test of this test operator should be considered suspect if they differ by mwe method in which 23 operators in 7 laboratories tested 6 than % Hegman unit (10 pm).; . v-.t samples of paints covering a broad range of compositions 9.1.2 Reproducibility--Two results, each the mean oftwg and finenesses, the single-operator standard deviation was readings, obtained by different operators in the same, of found to be 0.27 Hegman units (3.4 pm), the within-labo- diflEerpt laboratories, should be considered suspect if th?y; ratory standard deviation was found to be 0.70 Hegman units (8.8 pm) and the between-laboratories standard-devia- diffe"r by moire.th.a.n.2'./4.H^man uni.ts.(2.5 pm). rf' tion was found to be 6.74 Hegman units j^.3 pin,). Based on lfc Index Terms 2 Supporting data available fibm ASTM Headquarters. ' Request RRr D01-1017. i.;. /. lO.lTKfe test method iS indexed:tinder^theIfeBoftp terms: pigment dispersion (paint); fineness ofgrind (dispel sion);Hegman'scale. 150 DUP0502 97333 D 1210 -*4n} -100 -75 -50 -25 -O 3 Hegman 60pm Cleanliness Bating A - FIG. 4c Typical Fineness Gage Pattern . 4Hegman - 50pm Cleanliness. Rating B FIG. 4d Typical Fineness Gage Pattern 151 DUP050297334 D 1210 4 5 Hegman Cleanliness Rating C 35 tun FIG. 4e Typical Fineness Gage Pattern f 6 Hegman Cleanliness Rating B 25 pm FIG. 4g Typical Fineness Gage Pattern < 152 DUP050297335 -100 -75 -50 25 0 am -75 50 25 <Ql D 1210 7 Hegman Cleanliness Rating A 10 jun FIG. 41 Typical Fineness Gage Pattern TheAmerican Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 79703. 153 DUP050297336 <1 Designation: D 1211-87 f Standard Test Method for Temperature-Change Resistance of Clear Nitrocellulose Lacquer Films Applied to Wood1 This standard is issued under the fixed designation D 1211; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers determination of the resist ance to checking and cracking of clear nitrocellulose lacquer films applied to wood or plywood substrates when subjected to sudden changes from high to low temperatures. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 805 Testing Veneer, Plywood, and Other Glued Veneer Constructions1 2 D2571 Guide for Testing Wood Furniture Lacquers3 3. Description of Terms Specific to This Standard 3.1 True cold-checks on solid wood show as one or more straight cracks on the applied film. Cold-checks manifest themselves in either of two ways: 3.1.1 Long continuous wavy lines with the grain or at various directions at angles that can be perpendicular to the direction of the grain. 3.1.2 Innumerable fine lines erratic in direction an<F length forming a network over a portion or all of the panel. This effect may be likened to crazing of the lacquer film. 3.1.3 On plywood the direction of the cracks will oflen vary because of the stresses set up by other than the top stratum. Therefore, all checks may be considered as failures, and appropriate notations on the character of the cracks must be made to assist in the interpretation. While it is recognized that cracks in the substrate may occur (veneer checking), failures observed in the lacquer coating may be due to action of moisture (humidity) or of cold, or both. Checking caused by moisture appears along the grain and is characterized by short cracks (usually not more than `/z in. (13 mm) in length) occurring either singly or in clusters. These lines or clusters may progress along the grain in a discontinuous fashion. Should either veneer checking or 1 This test method is under the jurisdiction of ASTM Committee D-1 on Faint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO1.55 on Factory-Applied Coatings on Preformed Products. Current edition approved May 29, 1987. Published July 1987. Originally published as D 1211 - 52. Last previous edition D1211 -74(l980)el. 2 Discontinued; see 1975 Annual Book ofASTM Standards, Part 22. 1 Annual Book ofASTM Standards, Vol 06.01. moisture checking be observed, the test should be discon tinued, and rerun. 3.2 The checks may be perceptible only by visual observa tion of the panels at an angle, under a strong light, or the cracks may be wide enough to be readily discernible in direct daylight. 4. Summary of Test Method 4.1 Lacquer-coated wood panels are subjected first to a high temperature, followed by an exposure to low tempera ture, and then a return to room temperature for given periods of time, which constitutes one cycle. The method does not define the number of cycles which a lacquer must withstand, this condition being a requirement which must be agreed upon by the purchaser and the seller. 5.. Significance and Use 5.1 A common type of failure of clear films applied to wood is cracking or checking that may occur over a period of time either with the grain or at an angle. This cold check test is designed to accelerate, the appearance of checks or cracks by cycling the temperature; N' 1--Except when elaborate precautions are taken to control the moisture content.of the wood:before and after finishing and during the test, failures may quite often occur as a result ofdimensional changes in the wood due to moisture change rather than temperature change. 6. Apparatus 6.1 Refrigerator (Dry Ice)--The refrigerator should be a well-insulated box, cooled by air which has been circulated over solid carbon dioxide (dry ice). The air must strike the panels indirectly after passing over the solid carbon dioxide. The unit shall have a capacity and temperature control sufficient to cool the test panels in accordance with the requirements prescribed in Section 9. 6.2 Mechanical Refrigerator--As a less desirable alterna tive, a well-insulated mechanical refrigerator may be used having sufficient capacity to cool the test panels in accord ance with the requirements prescribed in Section 9. The refrigerator should have some means for providing ait circulation. It should be understood that results obtained with a mechanical refrigerator may not correspond to results obtained with a "dry ice" refrigerator. Consequently the type of unit employed shall be stated in the report. 6.3 Oven--The oven shall be electrically heated and of any standard type capable of being automatically controlled and of sufficient capacity to heat the panels under test to 1$ 5'F (49 3C) within 1 h. A circulating fan shall 1* installed in the oven. fro: bac sizi test app 7 ofv Typ rept 7. not testi min Met 7. to 8 | 8. P ; 8.i straip other 8.1 or eq 8.1 allow 8.1 thick) pericx 13 p.n not ec 8.1. apply of eac aging only the dc No t the size 8.1.. deternr panel measu: magne and ru be clos ,results Practio 8.2 CompU Purcha: 4 These Handbook 15.4 DUP050297337 e discon* observalt, or the in direct first to a tempera:or given : method uer must 1 must be pplied to period of :heck test or cracks control the during the changes in tange. uld be a irculated trike the dioxide, control with the e aiteraa' be used n accordn 9. The iding air obtained to results y the type :d and of ;ontrolled estto 120 t shall be D1211 7. Test Panels 7.1 Unless otherwise agreed, the test panel shall be cut from synthetic resin-bonded, five-ply plywood with feces and backs made with straight-grain walnut veneer having no sizing or other surface pretreatment. The dimensions of the test panel shall be 6 by 12 in. (152 by 305 mm), and approximately u in. (8 mm) thick. 7.2 Solid wood, heavier or lighter veneers, or other species of wood may be agreed upon by the purchaser and the seller. Type of wood and panel size should be clearly defined in the report. 7.3 The wood selected shall have a moisture content of not less than 6.0 % and not more than 8.0 % at the time of testing. The moisture content of the wood may be deter mined by an electric moisture gage or in accordance with Methods D 805. 7.4 Panels may be conditioned to a moisture content of 7 to 8 % under any of the following conditions:4 Temperature, F Relative Humidity, % 65 to 75 90 to 100 120 to 125 35 to 40 40 to 45 45 to 50 8. Preparation of Panels 8.1 Five-Ply Plywood (With faces and backs made with straight-grain, closed face walnut veneer having no sizing or other surface pretreatment) shall be prepared as follows: 8.1.1 Sand panels until smooth with No. 240 sandpaper, or equivalent. 8.1.2 Fill with representative walnut wood paste filler and allow to dry for 24 h at not less than 70 nor more than 80F. 8.1.3 Spray a sufficient number of coats of about equal thickness of the test lacquer on the panel within an 8-h period to give a total dry film thickness of 3 0.5 mil (75 13 tun). Allow a minimum period of 2 h between coats. Do not edge or back the panel with any protective coating. 8.1.4 To minimize the effects of variations in the wood, apply a control lacquer of known performance to a portion of each panel in the same manner as the test lacquer. After aging, the panels may be cut (Note 2) into sections finished only with one lacquer, but each section should conform to the description given in Section 6. N' 2--Cutting of panel is optional and may be contingent upon the size and capacity of the test equipment 8.1.5 The thickness of films applied to panels may be determined with reasonable accuracy by placing a metal panel adjacent to the wood panel being prepared and measuring the film thickness on the metal panel with a magnetic thickness gage. The plywood panel must be sanded and rubbed before testing and the use of waxes or oils should be closely regulated since these can make a difference in the results obtained. For sanding and rubbing procedure, see Practice D2571. 8.2 Panels of Five-Ply Plywood with Walnut Veneer for Complete Lacquer System--Proceed as agreed upon by the Purchaser and the seller. 1 These conditions were taken from the curve on p. 191 of the Wood Handbook, Forest Products Laboratory, Madison, WI. 8.3 Panels ofSolid Wood, Lighter or Heavier Veneers, or Other Species of Wood--Proceed as agreed upon by the purchaser and the seller. 8.4 General Treatment--Except where specific agree ments exist between the purchaser and the seller, all panels shall be subjected to the following treatment: 8.4.1 Prepare at least three panels for each lacquer or lacquer system and each other variable, such as type of panel, that may be under test. 8.4.2 Air-dry overnight. 8.4.3 Age finished test panels for ten days under condi tions that will maintain a moisture content of 6 to 8 %. 9. Procedure 9.1 Place a predetermined number of panels, depending on the capacity of the oven and refrigerator, vertically in racks so that air can pass between all panels. The lacquered sides of the panels shall not face the walls of the heating or cooling units. Place the racks for 1 h in an oven at 120 5F (48.9 3C) in such a manner as to avoid localized overheating. At the expiration of this period, transfer the panels within 1 min to a refrigerating unit maintained at --5 2F (-21 1C) (unless special conditions indicate some other agreement between the purchaser and the seller). The number of panels shall be such that the time required to reach this temperature is not less than 30 min and not more than 45 min. The temperature can be measured by a thermocouple imbedded in the panel just underneath the film. 9.2 Remove the panels from the refrigerator after 1 h exposure. After allowing 15 min relaxation period, inspect the panels under a strong light. Best results will be obtained if the light source is directed from behind and over the shoulder of the observer. Circle checks with crayon, since they will often heal or at least appear to heal and become relatively invisible. Once the capacity of any given ovenrefrigerator combination (number of panels that will permit specified rates of heating and cooling) has been determined, make all subsequent tests with this number of panels using dummy panels where necessary. If this precaution is not followed, rates of cooling and heating will differ each time the test is run, and reproducibility will suffer. 9.3 The period of 1 h at 120F (49C) followed by 1 h at -5F (-21C) and 30 min at room temperature (15 min relaxation period, 15 min to allow for inspection), constitutes one cycle. Repeat this cycle until failure occurs or until a prescribed minimum number of cycles has been obtained. 9.4 The failure end point is defined as the cycles on which innumerable fine lines appear as described in Section 3 or on which a total of four checks (1 to 2 in. (25 to 50 mm) in length) or two checks (more than 2 in. (50 mm) in length) appear in the film. Exclude the outer `/2-in. (13 mm) perimeter of panel when examining for failure (cracks). 9.5 Unless a laboratory operates on three shifts there will be a relaxation period every night and over week ends. The report should show when these rest periods occurred. 10. Report 10.1 Report the following information: 10.1.1 Type of construction, variety, and size of wood panels used, for example, 5-ply, Vie-in. (8-mm) walnut 155 DUP0502 97338 # D 1211 A veneer, 6 by 12 in. (152 by 305 mm), 10.1.2 Type of refrigerator, that is, "dry ice" or mechan ical, 10.1.3 Finishing system and schedule of application, and 10.1.4 Number of cycles passed without failure and note of all wood failures, specifying the cycle on which such failures occurred. 11. Precision 11.1 Results on all three panels should fall within 2 cycles of the mean of all three panels. If this does not occur, additional panels shall be run until there are at least three panels which fall within this range. All panels that have been run are to be taken into consideration. This requirement also applies to panels finished with the control lacquer. Precision as stated here applies only to the test panels described in Section 7. TheAmerican Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Itnot revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard ortoradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ! j | Y | | | ' 1. Scot 1.1 1 film thilacquer 1.1.1 (Englis! wet filir and up through 1.1.2 measurt (Sectior 1.2 7 safety p of who. appropr applical 2. Refe 2.1 A D823 Thi Tes 3. Sunn 3.1 T rigid tes The wet reduce f 3.2 h concent where t determi 3.3 Ir is pushe substrat< convex t from thi 4. Signi 4.1 VI tion of thicknes thicknes 'These paint and Subcommit Current Published a 2 Annua. 156 DUP05 0297339 a2 occur, : three ebeen at also vision bed in Designation: D1212 - 91 Standard Test Methods for Measurement of Wet Film Thickness of Organic Coatings1 This standard is issued under the fixed designation D 1212; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover the determination of wet film thickness of organic coatings such as paint, varnish, and lacquer. Two methods are described as follows: 1.1.1 In Test Method A, the Wet Film Thickness Gage (English or Metric graduation (see 5.1)) is used to measure wet film thicknesses up to 60 mils on the English scale series, and up to 700 pm on the metric scale series (Sections 5 through 8). 1.1.2 In Test Method B, the Pfund Gage is used to measure wet film thicknesses up to 14.2 mils (360 pm) (Sections 9 through 13). 1.2 This standard does not purport to address ifany, the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 3. Summary of Test Methods 3.1 The material is applied in the laboratory to plane, rigid test panels or in the field to the surface being coated. The wet film thickness is determined as quickly as possible to reduce shrinkage due to solvent loss. 3.2 In Test Method A, a gage with one eccentric and two concentric wheels is rolled over the surface and the point where the eccentric wheel first touches the wet film is determined. 3.3 In Test Method B, a gage with a convex lower surface is pushed into the wet film until the center touches the substrate. The diameter of the spot of wet coating left on the convex surface is measured and the film thickness calculated from the diameter of the spot and the radius of curvature. 4. Significance and Use 4.1 Wet film thickness measurements aid in the predic tion of dry film thickness. In instances where dry film thickness cannot be measured nondestructively, wet film thickness frequently specified. Also, the ability to deter ' These test methods are under the jurisdiction of ASTM Committee 0-1 on torn and Related Coatings and Materials and are the direct responsibility of Subcommittee DO] .23 on Physical Properties of Applied Paint Films. Current edition approved May 15, 1991. Published July 1991. Originally Published as D 1212 - 52 T. Last previous edition D 1212 - 85. ' Annual Book ofASTM Standards, Vol 06.01. mine wet film thickness during application can provide the opportunity to correct the application procedures. 5. Apparatus . TEST METHOD A 5.1 Wet Film Thickness Gage3--Two versions ofthe gage are now in use4: The original design as shown in Fig. 1 and a later design as shown in Fig. 2. Both designs consists of an eccentric center wheel supported by two concentric wheels so as to provide two scales that are bilaterally symmetrical. As the gage is rolled on the film, there is a change in clearance between the wet film and the eccentric wheel. The point at which the film first touches the center wheel measures the thickness of the film. 5.2 The later design shown in Fig. 2, moves the eccentric wheel from between the concentric wheels, as shown in Fig. 1, to the outside of the gage and closer to one of the concentric wheels. Gage reading errors of parallax across the gage are eliminated as the two scales are placed directly on the eccentric wheel and' errors when measuring on uneven support surfaces are reduced by placing the eccentric wheel closer to one of the supporting concentric wheels. 5.3 Best precision is obtained when using the near linear central portion of each scale, constituting about 80 % of its total fringe as shown in the diagram in Figs. 1 and 2. Therefore, the range of the particular gage selected for use should be such that the measured film thickness falls within, and preferably toward the center of the middle 80 % of each scale. Gages are available covering the following ranges in mils and microns; Range, mils O'to 2 Qto4 2 to 12 " 'iff to 30 20 to 60 Smallest Graduation, mils- 0.1 0.2 0.5 1.0 2.0 Range, pm Smallest Graduation, pm 0 to40 n9-to 100 5ffto 250 20016 700 Z0 5.00 10.00 25.00 3 Available from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Ln., Silver Spring, MD 20910 and from the Paul N. Gardner Company, Inc., 316 N.E. First Street, Pompano, FL 33060. 4 Both versions ofthis gage (Interchemical (INMOT) and Model "C"), available from BYK-Gardner, Inc., are covered by U.S. Patents 2 507 592 arid 3 128 558, and are held by Maynard R. Euverard, 113 Angail Town Ln., Williamsburg, VA 23185. Interested parlies are invited to submit information regarding the fdentificalion of acceptable alternatives to this patented item to the Committee on Standards, AaTftf Headquarter^ 1916 Race St, Philadelphia, 19103'. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. 157 DUP050297340 D 1212 i FIG. 1, Interchemical Wet Film Thickness Gages EXAGGERATED `VIEW OF THE POSITCONINQ OF THE OUTSIDE ECCENTRIC DISK ONTH604MIL RANGE GAGESHOWING A COATING THICKNESS ! FIG. 2 Model "C" Wet Film Thickness Gages 6. Procedure -. 6.1 Apply the material in accordance with Tfest Methods D 823 to suitable plane rigid panels ofarea sufficiently large to permit film thickness measurements at least 1 in. (25 mm) 8. Precision5 8.2 The 6.1 In an interiaboratory study of this test method, in proportion; which two operators in at least six laboratories maifc 1 measurements with the 0-- to 2- and 0- to 4-mil gages on three * -I '1 from any edge; Determine the film thickness immediately after application. :: 6.2 Support the test panels on a suitable level base in such a way that there will be no movement or spring of the panels during the film thickness measurements. Place the gage on the wet film so that the minimum marking is at the top and the greatest clearance between the eccentric wheel and the film is directly over the wet film. Roll the gage over the film one-half revolution in one direction toward the minimum marking on the gage and repeat in the opposite direction. materials, applied at two film thicknesses, the pooledwithia- laboratory standard deviation.was found to bed. 12 mils with 34 df and the between-laboratories standard deviation 0.18 for two determinations and 0.17 for four determinatidis with 25 df. Based on these standard deviations, the Moving criteria should be used for judging,the acceptability ofresufe at the 95 % confidence leydl: \ ' ~,Jt 8.1.1 Repeatability--Results? each the mean of opposiS rolls of the 0- to' 2- or 6- to 4-mil gage, obtained by the sahie 9. Apparai 9.1 Pfun convex lens of 250 mm an outer tul surface out applied to t film. The d of diameter Read the points at which the coating first makes contact with operator should be considered suspect ifthey;differ by mop D correspo. the eccentric wheel and determine the mean which is than 0.4 mil for two determinations and 0.5 mil for font the menisci considered as one reading. .................... determinations, .. ` on the glass 6.3 If the coating contains a- solvent that evaporates 8.1.2 Reproducibility--Two results, each the mean oft# 9.2 Steel rapidly or ifthe solids content is low, make at least a second separate determinations, obtained by operators in diffe0 millimetres. separate reading on a freshly applied film and calculate the mean of the separate readings. laboratories, should be considered suspect if they diffei more than 0.55 mil. 10. Procech io. i Apt 7. Report 7.1 Report the mean of the separate readings and the range and smallest graduation of the gage used. 5 Supporting data are available from A&TM Headquarters. ReflUtS D0I-I023. r Keinrath, ( `ethnology Cm 158 DUP0502 97341 ethod, in ies made s on three d withinmils with don 0.18 ninations following of results ' opposite the same r by more 1 for four ;an of two i different differ by Request RR; fi.Disia FIG. 3 PfundGage 8.2 The precision of higher range gages is expected to be proportional to film thickness. TEST METHOD B 9. Apparatus 9.1 Pfund Gage3--The gage6 shown in Fig. 3 consists of a convex lens L with lower surface having a radius of curvature of 250 mm mounted in a short tube Tu that slides freely in an outer tube T2. The compression springs S keep the convex surface out of contact with the wet film until pressure is applied to die top of T,, forcing the lens L down through the film. The displaced material forms an oversized circular spot of diameter D, on the convex lens (larger than the diameter D corresponding to the thickness T of the film) because of the meniscus effect due to wetting and surface tension effects on the glass lens. 9.2 Steel Scale (furnished with Pfund Gage), calibrated in millimetres. 10. Procedure 10.1 Apply the material to suitable plane, rigid panels of 6 Keinrath, G., "Sphere Penetration Gage," National Institute ofStandards and Technology Circular, NIST, Nat No. 585, Section 1.06, p. 4. area sufficiently large to permit film thickness measurements at least 1 in, (25 mm), from any edge. Determine the film thickness immediately after application. 10.2 Support the test panels on a suitable flat level base in such a way that there will be no movement or spring of the panels during the film thickness measurements. As shown in the second diagram in Fig. 3, place the gage on the coated surface and slowly force the inner tube down as far as it will go (point F on surface AB of the base) allowing displaced material to escape through the notches in the outer tube but preventing lateral motion of the gage. Upon releasing the pressure, an oversized circular spot is retained on the lens. Its diameter D is the length of the line EG and corresponds to the sum of. two thicknesses: AK = BC = thickness of underlying undisturbed coating: and KE = CG = thickness of overlying displaced coating. 10.3 Remove the gage from the surface, measure to the nearest 0,5 mm in two directions at approximate right angles the diameter of the oversize spot on the lens using the steel scale, and determine the mean of the two measurements that is considered as one reading. Make at least two separate tests to obtain the grand mean film thickness. 10.4 Although this procedure refers to measurements on flat test panels, the same technique may be used in the field or shop on commercial articles, provided the substrate is not distorted at the point of contact to an extent that would affect the measurements. 10.5 If coarse particles in the wet film prevent the lens from making contact with the base at the point F, the results will not be valid. 11. Calculation 11.1 The relations between the diameter of the oversized spot on the lens in millimetres, the approximate thickness of the undisturbed wet film, and the coverage in square feet per gallon are given in a printed table supplied with the Pfund gage. It has been found that empirical equations give approximate values for the wet film thickness, t, as follows: t (in mils) - (D2 x 1000)/16J? x 25.4 = 0.0943 D2 t (in micrometres) = (D2 X 1000)/16R = 0.25 & where: D = diameter of spot, mm, and R = radius of curvature of convex lens (250 mm), based on the fundamental assumption that t is exactly one half of the total thickness of the film at the diameter D, as shown in the second diagram in Fig. 3. 11.2 The Pfund gage cannot be calibrated by the manu facturer prior to delivery. For the best results, a correction factor must be established for each type and thickness of material, based on freshly prepared films of known wet film thickness, as measured by Test Method A (Interchemical Wet Film Thickness Gage). 12. Report 12.1 Report the mean of at least two separate readings as the wet film thickness. 13. Precision 13.1 In an interlaboratory study of this method, in which two operators in five laboratories made measurements on three materials applied at two film thicknesses, the pooled 159 DUP050297342 D 1212' s f I within-laboratory standard deviation was found to be 0.21 mil with 30 df and the between-laboratories standard devia tion with 24 df 0.285 mil for two measurements and 0.265 mil for four measurements. Based on these standard devia tions, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 13.1.1 Repeatability--Results, which are the mean of the two measurements at right angles, obtained by the same operator should be considered suspect if they differ by more than 0.6 mil for two determinations and 0.8 mil for four determinations. 13.1.2 Reproducibility--Two results, each the mean of two separate determinations, obtained by operators in dif ferent laboratories, should be considered suspect if they differ by more than 0.85 miL 14. Keywords 14.1 eccentric center wheel; glass panel reading surface; metals and metallic materials; paint coated panels; wet film thickness gage; wet film thickness measurement The American Society for Testing and Materials takesnoposition respecting the validity ofany patent rights assertedin connection with any Hem mentioned In this standard. Users of this standard are expressly advised that determination of the vaUdUy of any such patent rights, and the risk Of Infringement of such rightst are entirely their own responsibility. This standard la subject to revision at any time by the responsible technical committee and must be reviewedevery live years and Ifnot revised, etherreapproved orwHhdrawn. Yourcomments are Invtedetherlor revision of this standard or lorsddtional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration et a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should mske your views known to the ASTM Committee on Standards, 1916 Baca St., Philadelphia, PA 19103. 1. ho isl SU` sw at. ac. i th at at 2. 3. at as di & m 4. 160 DUP050297343 /jiflM Designation: D 1308 - 87 Standard Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes1 This standard is issued under tbe fixed designation D1308; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 6011, 6081 of Federal Test Method Standard No, 141A andfor listing in the D6D Index ofSpecifications and Standards. j. Scope 1.1 This test method covers determination of the effect of household chemicals on clear and pigmented organic fin ises, resulting in any objectionable alteration in the surface, such as discoloration, change in gloss, blistering, softening, ^veiling, loss of adhesion, or special phenomena. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. it is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D609 Methods for Preparation of Steel Panels for Testing Paint Varnish, Lacquer, and Related Products2 3. Summary of Test Method 3.1 Three test methods, each of which is particularly applicable to individual reagents under study, are described as follows: 3.1.1 Spot Test, Covered--The reagent is placed on the test surface and immediately covered with a watch glass. 3.1.2 Spot Test, Open--The test surface- is subjected directly to the effect of substance, such as citrus fruit, oils, greases, beverages, etc. 3.1.3 Immersion Test--A suitably prepared panel is im mersed in the test reagent. 4. Significance and Use 4.1 Resistance to various liquids used in the home is an important characteristic of organic finishes. These test methods provide the means by which the relative perform ance of coating systems may be evaluated. It should be recognized that continuous films are necessary for reliable results. 5. Test Panels 5.1 Steel Panels--See Method D 609. 1 This test method is under thejurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom nhtee DO1.55 on Factory-Applied Coatings on Preformed Products. Current edition approved May 29, 1987. Published July 1987. Originally Published as D 1308 - 54 T. Last previous edition D 1308 - 79 (1981)fl. 2 Annual Book ofASTM Standards, Vol 06.01. 5.2 Other Metal Panels, as agreed upon by the purchaser and the seller of the finish being tested. 6. Reagents 6.1 The choice of reagent shall be governed by ultimate coating use'and by agreement between the purchaser and the seller of the finish being tested. The following reagents are suggested: 6.1.1 Distilled Water, cold. 6.1.2 Distilled Water, hot. 6.1.3 Ethyl Alcohol (50 % volume). 6.1.4 Vinegar (3 % acetic acid). 6.1.5 Alkali Solution. 6.1.6 Acid Solution. 6.1.7 Soap Solution. 6.1.8 Detergent Solution. 6.1.9 Lighter Fluid and Other Volatile Reagents. 6.1.10 Fruit--Piece of cut fruit, with cut portion placed face down on panel for time agreed upon between the purchaser and the seller. 6.1.11 Oils and Fats--Butter, margarine, lard, shortening, vegetable oils, etc. 6.1.12 Condiments--Mustard, catsup. 6.1.13 Beverages--Coffee, tea, cocoa. 6.1.14 Lubricating Oils and Greases. 6.1.15 Other Reagents, as agreed upon between the pur chaser and the seller. 7. Procedure 7.1 Panel Preparation--Spot and direct application tests may be carried out on the fabricated article coated with the finishing system under evaluation, if sufficient plane surface is available. For immersion tests and tests where the finished article is not available, select panels in accordance with Methods D 609, or prepare special metal panels according to agreement between the purchaser and the seller of the finish. Apply the finish according to the method and the schedule prescribed by the user of the lacquer. This schedule includes number of coats, film thickness, and other features. Allow the finished panels to age 1 week at normal room conditions, about 77F (25C) and 50 % relative humidity, before testing. 7.2 Spot Test, Covered--Conduct the test at 73.5 3.5F (23 2C) and 50 5 % relative humidity, or as agreed upon between the purchaser and the seller. Using a 5-mL pipet graduated in 0.1 mL, pipet onto the horizontal panel 1 mL ofthe reagents listed in Section 6 and immediately cover with a watch glass. After an interval agreed upon by the 161 DUP0502 97344 # D 1308 purchaser and the seller, wipe the spot clean'and examine ately for any of the effects listed in Section 1. If desired, allow immediately for effects as listed in Section I. Frequently used the panels to recover for a specified period and examine for intervals are 15 min, 1 b, and 16 h, or by agreement between return of the original properties. In general, it will not be the producer and the user. If desired, allow the panel to necessary to seal the edges of the applied film. If the reagent recover for a specified period, and examine for return of original properties. 7.3 Spot Test, Open--Conduct the test at 73.5 3.5F (23 2C) and 50 5 % relative humidity, or as agreed upon effect is noted only around the panel edges, the test should be repeated using a suitable edge sealer. When sealing ofedges is required, the selection of the sealer should be a matter of agreement between the purchaser and the seller. between the purchaser and the seller. Place a small portion of the reagent on a horizontal panel or surface, with the exception of fruit juices, as mentioned in 5.1.10. After a time interval, as agreed upon between the purchaser and the seller, wipe the spot clean and examine immediately for effects as listed in Section 1. Frequently used intervals are 15 min, 1 h, and 16 h, or by agreement between the producer and the 8. Report 8.1 Report the following information: 8.1.1 System and the testing method employed. The test conditions are an important factor in the results obtained and, therefore, should be defined in the report. 8.1.2 The type of the effect, if any (see Section 1). user. If desired, allow the panel to recover for a specified 9. Precision and Bias period and examine for return of original properties. 7.4 Immersion--Immerse panels to a depth of 50 % in the 9.1 This test is designed to provide a working procedure for examination ofthe effect of household chemicals on clear specified reagents (6.1.1,6.1.2, 6.1.5,6.1.6,6.1.7, mid 6.1.8) and pigmentecforganic finishes. The effects will be in terms contained in beakers, at a temperature and length of time ,, of appearance, and numerical values are assigned if a rating agreed upon between the purchaser and the seller. Withdraw scale is used. Precision numbered values are not usually the panels, wash with distilled water, and examine immedi obtained for this type of qualitative test. The American Society for Tearing and Materials takes no position respecting the validity ofanypatent rights asserted In connection with any Item mentioned in this standard. Users of ttys standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any rime by the responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapproved or wkhdrewn. Your comments are Invitedeither forrevision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, tf you feet that your comments have riot received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. 1. Sr 1.1 simul paint 1.2 ation. addri the r. apprt applii sped! 2. Ri 2.1 D1 I 3. Si 3.1 both, to sir the p week; the v settlii of the 4. Aj 4.1 paini and . 4.: in. (1 in wi tip fr >Tb and Re mittee! Cun publish' 2 An 162 DUP0502 97345 red. allow amine f0p ili not be ie reagem should be ofedges is matter 0f The test obtained 1). procedure Is on clear J in terms if a rating )t usually Designation: D 1309 - 88 ! Standard Test Method for Settling Properties of Traffic Paints During Storage*1 This standard is issued under the fixed designation D 1309; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision A number in parentheses indicates the year of last reapproval. A superscript epsilon (r) indicates an editorial change since the last revision or reapproval. j, Scope I j This test method covers a laboratory procedure for mulating in 2 weeks the settling that might occur in traffic during approximately 12 months' normal storage. *(2 This standard may involve hazardous materials, oper as, and equipment. This standard does not purport to gldress all ofthe safety problems associated with its use. It is "lg responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a jpgcifjc hazard statement, see Note in 5.2. % Referenced Document 2.1 ASTM Standard: P869 Test Method for Evaluating Degree of Settling of Paint? j. Significance and Use 3.1 Paints, if not formulated or processed properly, or both, may settle excessively. This test method is an attempt to simulate the conditions that would accelerate settling of the pigment in order to evaluate settling properties within 2 weeks. The variables of this test method in conjunction with the very subjective method of evaluating the degree of settling (Method D 869) raise questions as to the usefulness ofthe results for specification compliance. 4.1 Container--Standard 1-pt (500-mL), friction top can paint container 3% `/is in. (85.5 1.5 mm) in diameter and Vk '/is in. (98.5 1.5 mm) in height. 4.2 Spatula, weighing 45 1 g with square-end blade 4% in. (125 mm) in length and approximately ,3/is in. (20 mm) in width. A suitable spatula may be prepared by cutting the tip from an ordinary 5-in. (125-mm) flexible steel laboratory 'This test method is under the jurisdiction ofASTM Committee D-l on Paint ffid Related Coatings and Materials and is the direct responsibility of Subcomniitee D01.44 on Traffic Coatings. Current edition approved March 23, 19SS. Published May 1988. Originally Wbfished as D1309 - 54 T. Last previous edition D1309 - 83el. 1Annual Book ofASTM Standards, Vol 06.01. spatula to the specified length. 4.3 Freezer, maintained at from --5 to --10F (--21 to --23.3C). 4.4 Oven, maintained at 160 2F (71 1C). 4.5 Lid Clips. 5. Procedure 5.1 Thoroughly mix the paint to be evaluated to a homogeneous consistency. Transfer enough of the paint to a 1-pt (500-mL) paint can to fill it to within Vi in. (13 mm) of the top. Close the can tightly, securing the lid with four clips, and subject it to the following exposure cycle. 5.1.1 Monday through Friday: 5.1.1.1 Place in freezer at 8:00 a.m. 5.1.1.2 Transfer to oven at 10:00 a.m. 5.1.1.3 Transfer to freezer at 2:00 p.m. 5.1.1.4 Transfer to oven at 4:00 p.m. 5.1.2 From 4:00 p.m. Friday until 8:00 a.m. Monday: 5.1.2.1 Place in die oven at 4:00 p.m. Friday. 5.1.2.2 At 8:00 a.m. Monday morning, after the can has been in the oven over a weekend, place it in the freezer and continue the cycles described above for another 7 days. Each time the can of paint is removed from the oven give it one sharp "spank" on the table top. The spank consists of a short rapid jar of the bottom of the can of paint against the top of the table. The violence ofthe jar is such that if the bottom of the can of paint were spanked against the platform of a scale instead of a table top the scale would register approximately 5 lb (2.27 kg) weight. 5.2 At the completion of the exposure, allow the paint to cool at room temperature for 4 h and determine the degree of settling in accordance with Method D 869. N' : Warning--Open cans slowly and carefully to allow release of residual vapor pressure. 6. Report 6.1 Report the "accelerated settling rating" in accordance with the degree of settling scale given in the Procedure section of Method D 869. 7. Precision and Bias 7.1 A round robin has been completed and precision and bias statements are being generated. 163 DUP050297346 D 1309 The American Society for Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users ofthis standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, am entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved orwithdrawn. Tour comments are Invited either for revision of this standard or for additional standards and should fie addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Race St., Philadelphia, PA 19103. 1.; 1 mij grii fini trat 1 fin< gru api ink T pm DJ cov ati ad the ap ap fa u.: le 164 DUP050297347 Designation: D 1316 - 87 Standard Test Method for Fineness of Grind of Printing Inks By the NPIRI Grindometer1 This standard is issued under the fixed designation D 1316; the number immediately following the designation indicates the year of original adoption or, in the ease of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. j. Scope 1.1 This test method describes the procedure for deter mining the fineness of grind of printing inks using a NPIRI grindometer. It evaluates the size of the largest particles in a finished dispersion but not average particle size or concen tration of sizes. 1.2 This test method is applicable to any dispersion that is fine enough to fall within the 0-25 pm range of the specified grind gage. With a minor variation in procedure, it is applicable to both paste (nonvolatile) and liquid (volatile) inks. , ^, N' 1--The 0-25 pm gage specified in this test method is similar in principle to the 0-100 pm Hegman gage described in Test Method D 1210. Sieve analysis for concentration of particles above 45 pm is covered in Test Method D 185. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish' appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D185 Test Method for Coarse Particles in Pigments, Pastes, and Paints2 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems3 E 691 Practice for Conducting an Interlaboratory Test Study to Determine the Precision of Test Methods4 3. Descriptions of Terms Specific to This Standard 3.1 fineness of grind---a measure of the size and preva lence of oversize particles in a printing ink dispersion. 3.2 scratch--a depression at least 10 mm in length in the surface of a grind gage drawdown. A scratch develops when a particle (or agglomerate) is trapped between the blade acid die bottom of the path and is drawn along by the blade. 3.3 speckle--protuberance of particles above the surface' of a grind gage drawdown. Speckles occur at gage depths greater than those at which scratches occur and are caused by 1 This test method is under thejurisdiction of'ASTM Committee D-l on Paint >d Related Coatings and Materials and is the direct responsibility of Subcomittee D01.56 on Printing Inks. . Current edition approved Nov. 7.7, 1987. Published January 1988. Originally hhied as D 316 - 54. Last previous edition D 1316 - 68 (1979). 1Annual BooknfASTM Standards, Vols 06.01- and 06:02. ;.................... 1 Annual Book ofASTM Standards, Vol 06.01. * Annual Book ofASTM Standards, Vols 06.03,08.03, and 14.02. oversize particles that are not hard enough or of the proper size to produce scratches. 4. Summary of Test Method 4.1 This test method utilizes a grind gage having two precision machined grooves each 1 in. (25.4 mm) wide and with a 0-1 mil (0-25 pm) taper. The test specimen is drawn down the paths slowly if a nonvolatile (paste) ink, briskly if a volatile (liquid) ink. The drawdowns are examined for the scale readings at which four and ten scratches appear and at which a preponderance of speckles disappear. The mean of readings from four paths constitutes a single determination. 5. Significance and Use 5.1 Oversize particles in a printing ink may damage a printing plate and adversely affect the appearance of printed ink films. Fineness of grind measurements are useful for deciding when to stop the dispersion process and for deter mining if the test material meets specifications as agreed upon between the supplier and the customer. 5.2 Speckle endpoints identify the size of the largest particles in a finished printing ink. They provide a better measure of overall dispersion quality than do scratch endpoints but, while their single-operator precision is better, their between-laboratory precision is far poorer. 5.3 Scratch endpoints indicate the size and relative number of the coarsest hard particles in a finished printing ink. They provide a measure of grittiness; the higher the 4-scratch endpoint, the grittier the ink; the smaller the difference between the 4- and 10-scratch endpoints, the larger the number of gritty particles in this range. Scratch endpoints may, however, miss gritty particles that ride in the bank ahead of the scraper; for this reason, they are not recommended for premixes or other dispersions containing a preponderance of gritty particles. 6. Apparatus 6.1 NPIRI Grindometer,5 consisting of a block of hard ened steel5 1 in. (25 mm) in thickness,6 3 Vi in. (89 mm) in width and 9 Vi ini (240 ham) in length. The top surface of the block is precision, machined so as to contain two paths, each 1 in. in width, 6 Vi in. (165 mm) in length, and' tapered uniformly in depth lengthwise from 1 mil (25 pm) to zero depth. Depth markings are inscribed on the shoulders at each 0.1 mil (2.5 pm) change in taper. Scale inscriptions and the 5 The NPIRI Grindometer, developed by the National Printing Ink Research Institute, may be obtained from the Precision Gage and Tool Co., 28 Voikenand Ave., Dayton, OH 45410. 6 Also available is a model 0.918 in. (23.3 mm) in thickness, which may serve as a type-high printing plate in a flat-bed press. 165 DUP050297348 D 1316 TABLE 1 Relation Among Grind Gage Scales No t ' --gu--NPIRI grindometer unit. NPIRI Scale/ gu 0 1 2 3 4 5 6 7 8 9 10 Depth mils- nm 00 0.1 2.5 0.2 5 0.3 7.5 0.4 10 0.5 12.5 0.6 15 0.7 17.5 0.3 20 0.9 22.5 1.0 25 ,, Micrometer jim 0 5 10 15 20 25 Hegman . Scale ;- 8 7 6 , 15 1.5 30 20 2.0 50 25 - 2.5 ' 63 30 3.0 75 35 3.5 68 40 4.0 100 50 75 100 5 4 32 1 0- * Numbers above dashed lines are Inscribed on the side or on the left shoulder of all standard NPIHI Grfndometers. Numbers below dashed lines represent 'extended scales available on special gages: e Nominal depth, not necessarily thickness of material deposited in paths of grind gages. Path tillage Is about 80 % for a high viscosity (sheet-fed offset) ink; 60 % for a low viscosity (letterpress news) ink. Path Ullage is also decreased by fast' drawdowns. c Numbersabove dashed lines are inscribed at every fifth calibration line on the right shoulder of newer NP1RI Grindomefers. 0 Paint Scale in Test Method D1210. relationship among various scales are given ifi Table 1. 6.2 Scraper,7 a double edged blade conforming to Test Method D 1210. '< 6.3 Ink Knife, small. Li 7. Materials 7.1 Rags or Tissues, lint- and metal-free. 7.2 Solvent, naphtha or other as appropriate for the ink under test 8. Care of Gage and Blade 8.1 Cleanliness--The scraper and the block must he, perfectly clean prior to a drawdown. Any dirt or lint present may produce a scratch and give a false reading s' Misuse--The grindometer is a precision instrument and must be treated as such. Do not let any hard materials contact the gage surface or scraper in any manner thapmight result in scarring or nicking. Avoid tapping or scratching with other metal. Use only soft metal-free cloths for cleanup. 8.3 Normal Wear--Under steady usage over an extended period oftime, both scraper and block will wear but idealized, scraper wear is much more rapid than block wear. Periodi cally check the blade as follows: ; 8.3.1 Method 1--Place a small quantity of'an ink across one end of a flat glass plate and make a drawdown. A uniform drawdown indicates that the particular scraper edge is in good condition. A streak of ink or a heavier film of ink at the places corresponding to the shoulders of the 7A second scraper should be procured for use while the first scraper is being reconditioned or is otherwise out of commission. grindometer is evidence of blade damage or excessive wear. Repeat the drawdown with the other edge of the blade. 8.3.2 Method 2 (from Test Method D 1210)--Face one edge ofthe scraper down across the bottom ofthe top surface of the grindometer or Other smooth level surface. Place a strong light behind the scraper and examine the contact edge; any light coming through shows that the blade edge has been damaged and is not satisfactory for use. Wear and warpage can also be detected by rocking the blade back and forth. Repeat the procedure on the other edge of the blade. 8.4 Rusting--The grindometer is made of carbon steel and is subject to rusting. Apply a coating of grease or other rust-preventative and keep covered or encased when not in use. N' 2: Caution--Do not use a gage or blade that exhibits damage or wear (see 8.2. to. 8.4). Replace or return to the manufacturer for reconditioning. ; 9. Sampling ' 9.1 Approximately 2 to 3 mL of ink sample is sufficient to fill four paths of the grindometer. When taking samples either from a container or from a disperser, push aside the top layer and take the sample from below. This technique prevents skin or surface dust from Being transferred to the ' gage. 9.2 If the sample, is a liquid ink, hand stir the sample vigorously for 2 min, taking care that air bubbles are not " whipped in. 10. Procedure 10.1 Place the gage on a flat, non-slippery surface so that, the deep end of the grooves is farthest from the operator." Wipe clean immediately before the test. Be sure die gage surface is dry and free of lint and wipe marks. 10.2 Using the ink knife, transfer a small quantity ofink across the deep end of both grooves about Vi in. (12.5 mm) from the end of the block. Alternatively, different inks may be placed in the two respective paths. . 3 , 10.3 Grasp the scraper in both hands and, holding in a 1 vertical position, place it behind the ink of the gage. Apply adequate pressure to ensure positive, contact of the bl^derj with the surface ofthe gage and chaw the ink down the length 1 of the path. Ink remaining on the shoulders is evidence bfj| insufficient,pressure. ' 10.3.1 Paste Inks--Makfe the drawdown with`a smopijl steady stroke tha^ takes 7 to 10 s to complete. 10.3.2 Liquid Inks--Make the drawdown with a stroke that takes .1 to 2 s to complete. When testing i inks, it is essential to work quickly, as partial drying ofl ink specimen or the ink film can influence test results.`.T 10.4 Set the blade on a sheet of scrap paper, and ihlnt ately pick up the gage to read the endpoints. Rotate th< in a light until the patterns, when viewed from the si<j clearly visible. Record endpoints (see Section 11) within?* 10 s of completing the drawdown. 10.5 Immediately clean the gage and repeat the pr< in 10.2 through 10.4 until readings have been made op paths per sample. If a reference standard was used in. c path, alternate its position on the repeat tests; 166 11 sea roui DUP050297349 t' v ..-t save wear blade. -Face 0ne top surface * Place! 'ntact edge. iehasbeea td warpage and forth ide. irbon steel se or other hen not jj its damage or ufacturer f0r ufficientto tg samples h aside the technique rred to the the sample les are not i D 1316 ai 2 Precision of QrindometerEndpoints for Roll-Milled l*8 Dispersions gndpows DSetavniadtaiornd. gu naorees oDf eFgrereeedsom Maximum Allowable 'Difference, gufppi) A. Repeatability (single operator; ^scratch ^scratch 0.31 0.27 0.15 36 36 30 0.87 (2.2) 0.76(1.9) 0.43 (1.1)* 8. Reproducibility (between laboratories) ^.scratch (O-scratcn 9*C*K>S ''ieTriparable figures 0.72 Q.70 1.97 from the precision 30 30 24 statement of Test 2.1 (5.0) 2.0 (5.0) 5.6 (14.2)* Method D1210 are ' , ^^^^peatability and 25 pm tor reprodueibiiity. jl Reading of Endppints and Report jl i Read the following endpoints to 'h gu (see NPIRI ^jle jn Table 1) or to 1 |xm or both. >_< The first point from the deep end at which four each at least 10 mm long, occur simultaneously, pie scratches need not reach the bottom ofthe plate groove. 11.1.2 As in 11.1 for ten scratches. 11.1.3 The place at which speckles disappear. 11,2 Record the three types ofendpoints on a total offour jaths and compute the respective means. [1.3 When reporting endpoints, mean figures may be funded to 'h gu, or to 1 pm, or both. 12, Precision and Bias8 12.1 Precision: 12.1.1 An- interlaboratory study of this test method was conducted in which one operator in each of seven laborato ries made two determinations, each the mean ofreadings on four drawdowns, on two different days on six carbon black dispersions. The samples represented two different levels of premixing, each followed by one, two, or four passes on a roll mill The results were analyzed statistically in accordance with Practice E 691. On the basis of the standard deviations shown in Table 2, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 12.1.T.1 Repeatability--Two results, each the mean of readings on four drawdowns, obtained by the same operator should be considered suspect if they differ by more than the scale readings given in the last two columns of Table 2, Section A.- 12.1.1.2 Reproducibility--Two results, each the mean of readings oh four drawdowns, obtained by operators in different laboratories should be considered suspect if they differ by more than the scale readings given in the last two columns of Table 2, Section B. 12.2 Bias--Bias cannot be determined as there is no standard material. In the interlaboratory study described in 12.1.1, speckle endpoints were more sensitive to expected differences in degree of dispersion than were scratch endpoints. face so that e operator, re the gage ntity of ink (12.5 mm) it inks may tiding in a ige. Apply the blade the length vidence of i a smooth ith a brisk esting fluid tying of the esults. nd immedi ate the gage :he side, are within 5 to a Supporting data are available from ASTM Headquarters. Request RR: D01-1054. The American Society for Testing and Materials takes noposition respecting the validity of anypatent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, and the risk ot infringement ot such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, either reapproved or withdrawn, Yourcommentsare Invited eitherfor revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters, Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. V. 1*.- 167 DUP0502 97350 !J|Jj Designation: D1360 - 90a T Standard Test Method for Fire Retardancy of Paints (Cabinet Method)1 This standard is issued under the fixed designation D1360; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 5. Significance and Use 1.1 This test method determines quantitatively the fire retardant properties ofa coating or coating system on a wood surface and the leaching effect ofwater on the fire retardancy of the coating or coating system. Specifically, this test method determines the weight loss and char index of coated panels subjected to a flame and the effect of leaching ofthe coating on these parameters. 1.2. This test method should be used solely to measure and describe the properties of materials, products, or systems in response to heat and flame under controlled laboratory conditions and should not be considered or used for the description, appraisal, or regulation of the fire hazard of materials, products, or systems under actual fire conditions. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 5.1 This test method determines the relative fire-retardant properties of coatings and the water leaching of the fireretardant material from the applied coating. Leaching simu lates the effect ofhigh humidity, weathering, and washing on the fire retardancy of a coating, and is specified in various regulations and specifications for fire-retardant paints. 6. Apparatus 6.1 Cabinet3--A glass and metal box as shown in Fig l, - 6.2 Assembly,3 consisting of supports for the test panels and solvent cup. The assembly is shown within the cabinet in Fig. 1. 6.3 Cylindrical Cup, to hold solvent, made of brass to the following dimensions: Outside diameter, in. (aim) Outside height, in. (mm) Wail thickness, in. (mm) Volume, mL Operating capacity, mL 'Vis (24) "At (17) On (1) 6.0 5.0 2. Referenced Documents 6.4 Balance, weighing to 0.1 g. 2.1 Federal Standard:2 Fed Spec. TT-V-119--Varnish, Spar, Phenolic Resin 6.5 Buret orPipet, calibrated in millilitres. 6.6 Container or Water Bath, 12.5 by 6.5 by 6.5 in. (320 2.2 Military Standard:2 Mil Spec. MIL-A-22397--Adhesive, Phenol, and Resor- by 165 by 165 mm), galvanized steel with cover to accom modate 15 panels, or other sizes to accommodate 5 to 10 I cinal Resin Base for Marine Use panels. 6.7 Oven capable of maintaining a temperature of 120 "*: ! 3. Terminology 3F (50+ 2C). 6.8 Constant Temperature and Humidity Cabinet or (38 mm)' 3.1 Description of Terms Specific to This Standard: 3.1.1 fire retardancy, n--in paint, the ability ofa paint to retard the spread of a flame over coated substrate usually at Room, maintained at 50 5 % relative humidity and 73.5 3.5T(23 2'C). any one shall con be kiln d the sacrifice of the paint film. 7. Test Materials moisture 4. Summary of Test Method 4.1 Fire Retardancy--Panels are conditioned before and after coating with the material under test. They are subjected to a flame from a small amount of burning alcohol or other solvent and the weight loss and char index are determined. 4.2 Leaching--Similarly prepared panels are immersed in water for a specified time and then subjected to the fire* retardancy test. The weight loss, char index, and difference in weight loss and char index between leached and unleached panels are determined. 7.1 Ignition Fuel, absolute ethyl alcohol (ethanol) or comparable solvent blend. N' 1--A mixture of 71.4% reagent grade isopropanol and 28.6% reagent grade methanol having the same heat of combustion as pure absolute ethanol may be used as the source of ignition. 7.2 Test Panels: 7.2.1 Unless otherwise specified or agreed, yellow poplar heartwood panels Vt by 6 by 12 in. (6 by 150 by 305 mm), close-grain, and as nearly edge grain as possible, free from knots and other imperfections, with surfaces planed and weigh fro 7.2.2 I used whe per panel N' 2- steel, or cor and the sell, 8. Prepar 8.1 Cor phere of 5 sanded. Panels shall be of solid wood or edge glued sections 2"C) prior to obtain the width, provided that no strip is less than 1 'A in. 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint ji and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.22 on Health and Safety. coats of va condition) h. Current edition approved Oct 26, 1990. Published December 1990. Originally published as D 1360 - SS T. Last previous edition D 1360 - 90. 2 Available from Standardization Documents Order Dedc, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, ATTN: NPODS. 3 A suitable cabinet and assembly may be obtained bom Custom Scientific Instruments, Inc., 13 Wing Drive, Cedar Knolls, NJ, 07927. Drawings ofcabinet, assembly, etc., may be obtained from ASTM Headquarters. Order PCN 12413-600-14, 8.2 Bru ft2/gal (6 coats at 5C 168 DUP050297351 # D 1360 retardant the fireng simuishing on 1 various its. in Fig. 1. st panels abinet in ass to the 5 in. (320 :o accome 5 to 10 of 120 abinet or nd 73.5 land) or and 28.6 % don as pure >w poplar 305 mm), free from aned and d sections ml `Aid- sbisrs jl 12- View A FIG. 1 Apparatus VtewB (38 mm) wide and that no more than two glue lines occur in aay one panel. The adhesive used in glueing these panels shall conform to Mil. Spec. MIL-A-22397. Test panels shall he kiln dried so as to contain no more than 10.0 weight % moisture and after conditioning as specified in 8.1 shall I weigh from 27 to 30 lb/ft3 (125 to 140 g/panel). 12.2 Douglas fir or other woods shown in Table 1 may be ! used where required. Table 1 shows the densities and weight | per panel for each wood after conditioning. N ' 2--Asbestos board (or inorganic reinforced cement board), I or concrete may be used upon agreement between the purchaser | Wthe seller. * Preparation of Test Panels 8.1 Condition panels for 14 days in a controlled atmosj 50 . 5 % relative humidity and 73.5 3.5F (23 ; prior to coating. Seal the ends of the panels with two j ofvarnish conforming to Fed. Spec. TT-V-119 after the J&ditioning. Allow each coat of varnish to air dry 18 to 24 0. *2 Brush apply the material under test in one coat at 250 ,:M6 m2/L) (wet film thickness of 6.4 mils) or in two I'nwsat 500 ft2/gal (12 m2/L) (3.2 mils per coat) to each face of each panel, obtaining as uniform coverage as possible. Application can be by other conventional means and in as many coats to obtain the necessary weight of coating or desired wet or dry film thickness. Also coat the edges and sides of the panels with the same material. When applied in more than one coat, dry 24 h between coats under standard conditions (see 6.8) and, after the final coat, dry 14 days under the controlled conditions. Prior to subjecting the specimens to the burning test, place them in the oven at 120 3F (50 2*C) for a period of 40 h. 8.3 Calculate the weight of the coating to be applied using the following equation: where: W ' (6 x 12) 1445 D x 454 W = weight of applied wet coating, g, D = coating density, lb/gal, and S = spreading rate in ft2/gal. 8.3.1 Use the following equation when metric units are employed: W= (46.4Z))/5 where: 169 DU P050297352 # D 1360 La TABLE 1 Densities and PaneI Weights of Various Woods N!"' --Conditioned at relative humidity 50 5 % and 73.5 3.5F (23 2C) for 14 days. Type of Wood Density (9 to 10 weight % Moisture), Ib/ft3 (kg/m3) Weight of 6 by 12 by V* In. (152 by 305 by 6 mm) Panel, g Red cedar Douglas fir White pine-ponderosa pine Southern yellow pme Redwood 21.4-22.4(345-360) 29-35(465-560) 22.4-26.4 (360-420) 31-37(495-590) 27.2-28.2 (43S-450) 101-106 137-165 106-125 147-175 129-133 W = weight of applied wet coating, g, D = coating density, g/mL, and S = spreading rate, m2/L. 9. Procedure--Fire Retardancy 9.1 Assemble the apparatus as shown in Fig. 1, including the stack extension and downdraft hood, in an area where facilities are available for the removal or escape of combus tion products (standard laboratory hood without forced ventilation). Weigh the panel to be tested to the nearest 0.1 g and record the weight Center the panel, face down, on the angular supports with the lower edge 2 in. (50 mmjfrom the angle formed by the floor and the side wall of the cabinet. Place the fuel cup, at room temperature, on the pedestal so that the vertical distance from the cup lip nearest to the face of the specimen is exactly 1.0 in. (25 mm). Using a buret or pipet, add 5.0 mL of pure absolute ethanol or any mixture with the same heat of combustion (Note 1) to the cup and ignite without delay by means of a flame approximately Vi in. (13 mm) in length. Close the door and adjust the draft to assure complete burning of the alcohol. Allow the test to continue until all flames self-extinguish. Repeat this proce dure with at least five replicate panels. 9.2 Weight Loss--Cool each panel to room temperature and weigh to the nearest 0.1 g. Determine the weight loss in grams of each of the five specimens by subtracting from its original weight (see 9.1). Calculate the mean and standard deviation for the weight loss. If the standard deviation of the five replicates is greater than 10% of the mean, test five additional panels and calculate the mean weight loss of the ten panels. 9.3 Char Index--Cut the panels by means of a finetoothed saw along the lines of maximum length and width of attack. Measure in centimetres the maximum width of charring of the wood panel below the paint film on the lateral cut Likewise, measure the maximum length of charring found on the longitudinal cut. Measure the max imum depth to which charring has penetrated the wood as evidenced on the longitudinal or lateral cuts. Determine the, char index by multiplying the maximum char length, width, and depth figures. Calculate the mean and standard devia tion for the char index. If the standard deviation of the five replicates is greater than 10% of the mean, test five addi tional panels and calculate the mean char index on the basis of the ten panels. 10. Procedure--Leaching Test 10.1 Prepare, coat, and condition 15 panels of each material under test as described in Section 8. 10.2 At the end of 14 days at 50 % humidity and 73.5'F (23C), immerse the 15 panels in 2250 30 mL of water (150 mL/panet) (Note 3) for 40 h at 120 3F (50 2C). N#$' 3--The water bath is made to contain 15 panels and 2250 mL of water to cover the specimens. If less than 15 coated panels are immersed, add blank panels to make up the i5.- Place panels so that their faces do not touch. Cover the bath to prevent excessive evapora tion. >\ 10.3 Subject each' ofthe if panels to the fire retardant test in accordance with 9-1 and calculate the differences in mean weight loss and mean char index between the leached and the unleached set of specimens as follows: A wt. loss = mew wt, loss of leached specimens - mean wt. loss of unleached specimens. A char index -- mean char index of leached specimens -- mean char index of unleached specimens. 11. Report 11.1` Report the following infbmiation: 11.1.1 The number of coats and the coverage in ft2/gal (m2/L) of the total numbers of coats for each set of each material under test, 11.1.2 The mean weight loss and the mean char index of the set exposed only to the fire retardancy test, the number of specimens used in calculating the means, and the final standard deviation, and 11.1.3 The difference in mean weight loss and mean char index between the sets of unleached and leached specimens as determined in 10.3. 12. Precision and Bias 12.1 The precision of this test is to be determined. 12.2 Bias--The bias of this test method cannot be deter mined as the value of fire retardancy can be defined only in terms of a test method. 13. Keywords 13.1 cabinet method; char index; fire retardancy; govern ment specification; paint This test related fini: Formerly discontintu \ TheAmerican Society for Testing and Materials takes noposition respecting the validity ofany patent rights,asserted In connection with any Item mentioned In this standard. Users of this standard ere expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, ate entirely their own responsibility. : This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP0502 97353 \ Last ASTM Designation: D1395 - 58 (Reapproved 1974) gth, width, ard devia. of the five five addi. n the basis s of each ind 73.5'F - of water 0 2C). ad 2250 mL 1 panels are .nels so that ive evapora- ardant test ;s in mean ached and mean wt. :cimens -- Standard Test Method for Abrasion Resistance of Clear Floor Coatings i This test method covers the determination of the abrasion resistance of clear floor finishes such as lacquer, varnish, and ,elated finishes when applied to small test panels. Formerly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials, this test method was discontinued in 1989. 41 , .- in ft2/gai it of each r index of lumber of the final nean char specimens d. be deteri only in y, govern- a . ' ;.v * . . .. ji > ' _{.. . i i \, ' . ' " > . ; ,A . . .( - ' 171 ---------------- /I' ' * - * n. .. --- --------------------------------------- DUP0502 97354 <1! Designation: D 1400 - 87 Standard Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconducfive Coatings Applied to a Nonferrous Metal Base1 This standard is issued under the fixed designation D 1400; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the nondestructive measure ment of the dry film thickness of electrically nonconducfive footings applied over a nonferrous metal base using com mercially available eddy current instruments. 1.2 Ibis test method is not applicable to coatings that will be readily deformable under the load of the measuring instrument. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport toaddress all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 5. Apparatus 5.1 Eddy Current Thickness Gages, commercially avail able, suitable to measure coating thickness accurately.4 6. Test Specimens 6.1 When this test method is used in the field, the specimen is the coated structure or article on which the thickness is to be evaluated. 6.2 For laboratory use apply the materials to be tested to panels ofthe composition and surface conditions on which it is desired to determine the thickness. N%&' 1--Applicable test panel description and surface preparation methods are given in Practices D 1730. N%&' 2--Coatings should be applied in accordance with Test Methods D 823, or as agreed upon between the purchaser and the seller. 8 assi rest 8 ma; 8 acc int asst 8 the 8 imi mo: 8 isfi the the */i i 8 an < met spe< has 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting3 3. Summary of Test Method 3.1 Instruments covered by this test method measure coating thickness by the use of eddy currents. The instru ment probe must be placed directly on the coating surface to take a reading. 4. Significance and Use 4.1 The instrument probe coil is energized by alternating current which induces eddy currents in the metal substrate. The eddy currents in turn create opposing alternating magnetic fields in the substrate that modify the electrical characteristics of the probe coil. The extent of such changes is dependent upon the distance between the probe and the metal, the distance being shown on the instrument meter as the thickness (mils or micrometers) of the intervening coating. 4.2 The accuracy of the measurements may be influenced when made closer than 1 in. (25 mm) to an edge or 3 in. (75 mm) to another mass of metal. 1 This test method is voder the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.23 on Physical Properties of Paint Rims. Current edition approved May 29, 1987. Published July 1987. Originally published as D 1400 - 36. Last previous edition D 1400 - 81. 2 Annual Book ofASTM Standards, Vol 06.01. 1 Annual Book ofASTM Standards, Vols 02.05 and 06.01. 7. Calibration of Apparatus 7.1* Calibrate the instrument in an area free of stray magnetic fields, such as power lines, generators, or welding equipment. There shall be no vibration apparent on the test piece when the instrument is being calibrated. 7.2 Use a bare section of the substrate after the specified surface preparation method has been accomplished. If an uncoated section of the substrate is not available, uncoated test panels of a similar metal type over which the specified preparation has been performed may be used. 7.3 Use nonmagnetic thickness shims for calibration. Most shims are non-precision and therefore, thickness must be verified with a micrometer. 7.4 Select calibration shims in the expected thickness range to be measured. Ifa coating is expected to be 3 mils (75 pm) in thickness, calibrate the instrument at 3 mils. Then check the calibration using shims of both a lesser and greater thickness to determine the thickness range over which the instrument will register accurately. 7.5 Follow the manufacturer's instructions for the specific adjustment of the instrument. 8. Procedure 8.1 Use the instrument only after it has been calibrated in accordance with Section 7. 8.2 Assure that the coating is dry prior to use of the instrument. ' j Insta Af al CF 4 Apparatus found to be suitable include the Permascope, Dermitron, Minitest, and Minitector. Sources for the instruments are available from ASTM, 1916 Raw St, Philadelphia, PA 19103. DUP0502 97355 dally avail. ately.4 ; field, the which the be tested to on which it e preparation x with Test and the seller. ee of stray or welding t on the test he specified ished. If an e, uncoated he specified calibration, kness must i thickness ; 3 mils (75 mils. Then and greater . which the the specific D 1400 f inspect the probe tip and surface'to be measured to 0 that they are clean, otherwise erroneous readings can 8.8 Report the instrument used, serial number, range, and mean of thickness readings found. Take readings in areas free of vibration, electrical, or * -^fields. thickness readings are found outside the range of racy determined in 7.4, repeat the calibration procedure jCC:1ur - Check the calibration frequently during use to ''Lfj that the instrument continues to read properly. Take a suffitient number of readings to charatcterize diiegg 6.1 For laboratory measurements a recommended minJjjj is three for a 3 by 6 in. (75 by 150 mm) panel and fQje in proportion to size. g 62 For field measurements a recommended minimum five determinations at random for every 100 ft2 (10 m2) of L surface area. Each of the five determinations should be Jjj mean of three separate gage readings within the area ofa S in. (12 mm) diameter circle. g,7 Take measurements no closer than I in. (25 mm) to 0 edge or 3 in. (75 mm) to another mass of metal. If such measurements are necessary, recheck the calibration in the jpeeific area to determine the effect the edge or mass ofmetal ^son the instrument reading. 9. Precision 9.1 Precision--On the basis of an interlaboratory study of this test method in which eddy-current instruments from four manufacturers were used in several laboratories to measure a moderate range of dry-film thickness on the same set of panels, the within-Iaboratory and between-laboratories coefficients of variation were found to be as shown in Table 1. Based upon these coefficients the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 9.1.1 Repeatability--Two results obtained by the same operator using instruments from the same category should be considered suspect if they differ by more than the maximum allowable difference values given in Table 1 for the appro priate film thickness. 9.1.2 Reproducibility--Two results, each the mean of four measurements, obtained by operators in different laborato ries using instruments from the same category should be considered suspect ifthey differ by more than the maximum allowable difference values given in Table 1 for the appro priate film thickness. TABLE 1 Precision of Film Thickness Measurements -- Within Laboratory. Coating Thickness Degrees of Freedom (OF) 0.5 to 1.5 mils Coefficient of Variation {vw),% Maximum Difference {MAD), % ' Degrees of Freedom (OF) instrument: PermascopeEC Mlntest FN 250 28 3 8.7 .14 2 16 Minitest FN 250 4 6 Eicometer 150 FN 38 8 Dermitron 18- 8 Pooled 58 7.9 22.3 Between Laboratories Coating Thickness agrees of Freedom <DF) 0.5 to 1.5 mils Coefficient of Variation (Vj),* Maximum Allowable Difference (MAD). % Degrees at Freedom (DF) Permascope EC Bcometer 150 FN Pooled Minitest FN 250 Oemtitron 8 6 14 A A 3 5 3.98 12.1 A A 8 4 12 A A * Results are not provided. B Between-laboratories precision is usually larger than within-Iaboratory precision. 0 Percent relative precision is usually lower for thicker Sims. 3 to 3.5 mils Coefficient of Variation OO, % 2 2 2 A A 3 to 3.5 mils Coefficient of Variation (O, % 5e 3 4.44 Maximum Difference (MAD), 56 S.0 Maximum Allowable Difference (MAD), % 13.7 ralibrated in use of the nitron. Minitest, STM, 1916 Race The American Society tor Testing and Materials takes noposition respecting the validity ofany patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised thet determination of the validity of any suoh pedant rights, and die risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherraapprwedor withdrawn. Your comments are Invited either for revision ofthis standard or for additional standards end should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, ft you feel that your comments have not received a fairhearing you should make your views known to the ASTht Committee on Standards, 191b ftaco St., Philadelphia, PA 19103. m DUP050297356 a m 4 Designation: D 1474 - 85 (Reapproved 1991)1 Standard Test Methods for Indentation Hardness of Organic Coatings1 This standard is issued under the fixed designation D 1474; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (c) indicates an editorial change-since the last revision or reapprovaL These test methods have been approved for are by agencies of the Department ofDefense to replace Method 6212 of Federal Test MethodStandardNo. 141A. Consult theDoD Index ofSpecifications and Standardsfor the specific year ofissue that has been adopted by the Department ofDefense. t M'(' --Keywords were added editorially in January 1991. mIf .m #1 ri v / -* V !rI iS 1. Scope 1.1 These test methods cover the!'.determination of die indentation hardness of organic materials such as dried paint, varnish, and lacquer coatings, when applied to an acceptable plane rigid surface, for example, metal or glass. 1.2 Two methods are covered as follows: Sections Method A--Kitobp Indentation Hardiness ' Method B--Pfund Indentation Hardness 6 to 12 13 to 19 1.3 Method A, which has the greater precision, provides hardness values in terms of Knoop Hardness dumber (KHN). Method B provides hardness in terms of Pfund Hardness Number (PHN). Although the hardness value scales of these methods differ, the methods agree in the ranking of coating hardness. . 1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appro?. priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: .... D 823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Method for Nondestructive Measurement of Dry-Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 3. Terminology 3.1 Definitions: 3.1.1 indentation hardrms- -the resistance to penetration by an indenter. 1 These test methods are under the jurisdiction of ASTSi Committee D-Fon. Paint and Related Coatings and Materials and lire the direct responsibility of Subcommittee D01^3 on Physical Properties of ApplS^i Paint Films.-1 __ ...... Current edition approved Sept 27, 1985. Published Novemi>&'l985. Origmtilly published asD 1474 - 57 T. Last previous edition D 1474 - 68 (1979)*1. 2 Annual Book ofASTM Standards, Vol 06.01. 3.1.2 Knoop indenter--a pyramidal diamond of pre scribed dimensions. 3.1.3 Pfund indenter--hemispherical quartz or sapphire indenter of prescribed dimensions. 3.1.4 Krtoop hardness number, AHA/--the indentation hardness determined with a Knoop indenter, and calculated as follows: KHN = L/A,, = LjlxCp where: L = load applied to the indenter, kg, A = measured length of long diagonal of the indentation, ! mm, Cp -- indenter constant relating l2 to Ap, and Ap = projected area of indentation, mm2. 3.1.5 Pfund hardness number, PHN--the indentation! hardness determined with a Pfund indenter, and calculated ] as follows: PHN = L/A = ALjtcd2 = 1.27 (L/d2) where: L = load/kg applied to the indenter, kg, A -- area of projected indentation, mm2, and d = diameter of projected indentation, mm. 4. Significance and Use 4.1 Indentation hardness measurements have proven to| be useful in rating coatings on rigid substrates for theic| resistance to mechanical abuse, such as that produced blows, gouging, and scratching. These measurements do ao| necessarily characterize the resistance to mechanical abuse off coatings that are required to remain intact when deformed; 5. Test Specimens 5.1 The substrate for the coating shall be an accepta&l plane rigid surface such as glass or metal. 5.2 The coating thickness on any one panel uniform within 0.1 mil (3 pm). Coatings to be com] shall be of equal thfckneSs within 0,2^ mil (5 pm), maximum accuracy, the minimum permissible coal thickness shall be such that the depth of indentation does exceed three fourths of the coating thickness, to the effect of the substrate. ^ 5.3 At least three replicate specimens shall be tested each coating to be evaluated.- 5.4 Coatings should be applied in accordance with Methods D823 and their dry film thickness should 174 f< u DUP050297357 ,d of Dte. Jr sapphjjg indentation 1 calculated ndentation, indentation 1 calculated proven to . for their yduced by nts do not al abuse of deformed. , acceptable ,el shall be s compared 5 pm). For ble coating on does not o minimize jsted fr nth Test ouid be D 1474 in accordance with Test Methods D 1005, D 1186, pi*00' SViPTHOD A-KNOOP INDENTATION HARDNESS , Sonunary of Method ThjS method consists of applying a load to the surface ^mating by means of a pyramidal shaped diamond of jpecified face angles, and converting the measure^^of the resultant permanent impression to a hardness N)*' 3--The panel should be so mounted that it cannot move with respect to the stage in any direction during the course of the test. 9.3 Use the microscope to select an area of the test specimen that is free of surface irregularities and imperfec tions. Place this area under the indenter by means of the movable micrometer stage. N+,' 4--If good impressions cannot be obtained because of the roughness ofthe surface ofthe specimen, gently polish the surface with No. 400 carborundum and finish off with jewelers rouge before making the impression. i Hardness Tester,3 consisting of a load applicator, a 7,1 indenter, and a microscope fitted with a movable ^yjmneter stage- Tbe apparatus shall mechanically bring videnter into contact with the test surface with negligible & apply the selected full load, maintain it for 18 0.5 Wfrtttdnw the indenter. 5172 I(noop Indenter--The Knoop indenter is a pyramidal 1 with included longitudinal angles of 172 30' and "lauded transverse angle of 130" O'. -./' 1--The ratio of the long to the short diagonal of the impres- ' jj approximately 7:1; the ratio ofthe long diagonal to the depth of Creation is approximately 30:1. 73 Microscope--The microscope shall have a filar mi ster eyepiece and sufficient objectives to permit the measurement of the length of impression to within 1 %. jlte specimen shall be firmly supported on a movable micrometer stage attached to the microscope. g. Calibration 8.1 Adjust the illumination in the microscope to give fljirimnm contrast when viewing an indentation. 8.2 By means of a calibrated scale, determine the factor for each microscope objective that will convert the filar scale units of the eyepiece to millimetres. 8.3 With a 25-g load on the indenter, determine the KHN ofa calibrated standard (Note 2) whose assigned value is not greater than 50 KHN. Ifthe obtained value is within 5 % of the assigned value, the instrument is considered .to be inr calibration. N01' 2---A suitable source of calibrated standards in this hardness range is not available. Therefore, by agreement ofthe parties concerned, istable specimen (such as an aged coating of a baked enamel applied to t flat substrate) should be used to calibrate the participating hardness testers. 9.4 - Preset the apparatus to apply a 25-g load and perform the test according to the manufacturer's instructions. Main tain the.time the indenter is in contact with the specimen for 18 04 s. N23' 5--For maximum accuracy, care must be taken that the indenter does not penetrate the coating to a depth beyond three fourths of the coating thickness. This is necessary to eliminate any major substrate effect on the hardness measurement - 9.5 Immediately after the completion of the cycle, adjust the movable stage so that the indentation is in the field of the microscope. Focus the microscope on the indentation so that both extremities of the long diagonal (that is, where the upper edges of the indentation just converge) are as sharp as possible. Measure the length Of the long diagonal of the impression with the filar micrometer eyepiece. N45' 6--Select a microscope objective that will cause the length of impression to be between 200 and 800 filar units to assure maximum accuracy in measurement. 9.6 From the measurements obtained in 9.5, the informa tion given in Note 1, and the measured film thickness at the place of indentation, calculate the depth of indenter penetra tion. If the depth of penetration exceeds three-fourths of the coating thickness, the results may be influenced by substrate proximity. Therefore, for maximum accuracy it is desirable to prepare thicker specimens and repeat the test. Instead of this procedure, at the option of purchaser and seller, an indenter load of less than 25 g may be used. 9.7 Repeat the procedure described in 9.3, 9.4, and 9.5 until at least five impressions have been made at widely spaced locations on the specimen. 10. Calculation 10.1 Calculate the mean indentation length in filar units. 10.2 Convert this mean indentation length to KHN by means of the appropriate tables supplied with the instru ment. 1. Procedure N)*' 7--If a conversion table is not available, the KHN may be 9.1 Unless otherwise specified, make the hardnessr deter calculated as follows: i minations at 73.5 3.50F (23 2Q and 50 5 %-refaitive- "X , , KHN = 0.025H2C,, humidity after equilibrating the specimens under these' . where; > . conditions for at least 24 h. - 0.025 = load applied, kg, to the indenter, 9.2 Rigidly attach the specimen to the movable stage so / = length of long diagonal of indentation, mm, and the surface to be measured is normal to the direction of Cp -- indenter constant = 7.028 x 10~2. " dentation. 11.' Report *** (he hardness testers meeting the apparatus requirements ibr this the Tukon Micro-hardness Tester and the Riehle Kentron MicroJr"n'S5 Tester, available from the Page-Wilson Measurement System Div., 929 """teticut Ave,, Box 9021, Bridgeport, CT 06602. 11.1 Report the following information: -11.1.1 Mean and range of KHN values obtained for each specimen, stating the number of indentations made and the indenter load used; 175 DUP0502 97358 D 1474 11.1.2 Mean film thickness of each specimen, based on the measurements made at the points of indentation, 11.1.3 Specimen preparation and conditioning techniques used, and 11.1.4 Mean and range of KHN values of the replicate panels. 12. Precision 12.1 On the basis ofan interlaboratory test ofthis method in which operators in six laboratories tested seven coated panels having a broad range of hardness, the within-laboratory coefficient of variation was found to be 3 % with 21 degrees of freedom and the between-laboratories coefficient of variation 8 % with 30 degrees of freedom. Based upon these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 12.1.1 Repeatability--Two results, each the mean ofthree determinations on a specimen, obtained by the same oper. ator should be considered suspect if they differ by more than 9 % of their mean value. 12.1.2 Reproducibility--Two results, each the mean of three determinations on a specimen, obtained by operators in different laboratories should be considered suspect if they differ by more than 24 % of their mean value. j METHOD B--PFUND INDENTATION HARDNESS | [ 13. Summary of Method 13.1 This method consists of applying a load to the surface of a coating, by means of a transparent colorless quartz or synthetic sapphire hemisphere having a specified diameter, and converting the measurement of the resultant observed impression under load to a hardness number. 14. Appan 14.1 Ha method sh; sapphire in apparatus s be brought with neglig 14.2 Pfu transparent sphere wit! maximum 14.3 Mi crometer e measurer The specin stage. 14.4 Tit 0.5 s. WEIGHT SPRING LOADED HOLD-OOWN BUTTONS SAPPHIRE PENETRATOR FILAR MICROMETER MICROSCOPE LIGHT SOURCE ULTRQPAK ILLUMINATOR STANDARD TYPE CODE abtee ULTROPAK OBJECTIVE 3.01 CODE chpet BALL BUSHING LOCATING PLATE WEIGHT SUPPORT ADJUSTING SCREWS FOR CENTERING IMPRESSION IN. MICROSCOPE FIELD SPECIMEN CAM LEVER 15. Stands 15.1 Ad maximum 15.2 By for each m units oftfi 15.3 Wi PHN ofat not greate i 5 % of tl ered to be 16. Procei 16.2 Ur ruination; humidity, for not les 16.2 Ki such that direction 16.3 Vr the inden the full Io 16.4 A 1 measure t ; eyepiece c the diame the inden controlled 4 A hardm Pfund Indent; 1415 Park A\ FIG. 1 A Ptund Hardness Tester (Shown Before Application of Weight) 176 DUP050297359 ofthree* le oper>re than nean of perators t if they 5S to the colorless specified resultant cer. # D 1474 j4. Apparatus 14.1 Hardness Testers--The hardness testers used in this method shall consist of a load applicator, a Pfund quartz or sapphire indenter, and a. microscope fitted with a stage. The apparatus shall be constructed so as to permit the indenter to be brought manually into contact with the specimen surface with negligible impact. 14.2 Pfund Indenter*--The Pfund indenter (Fig. 1) is a transparent colorless quartz or synthetic sapphire hemi sphere with a spherical radius of 0.125 in. (3.18 mm) and a maximum spherical eccentricity of 0.002 in. (0.05 mm). 14.3 Microscope--The microscope shall have a filar mi crometer eyepiece and sufficient objectives to jpermit the measurement of the diameter of impression to within 1 The specimen shall be rigidly supported on the microscope stage. 14.4 Timer, capable of measuring a time interval of 60 : 0.5 s. 15. Standardization 15.1 Adjust the illumination in the microscope to give maximum contrast when viewing an indentation. 15.2 By means of a calibrated scale, determine the factor for each microscope objective that will convert the filar scale units of the eyepiece to millimetres. 15.3 With a 1.0-kg load on the indenter, determine the PHN of a calibrated standard (Note 2) with an assigned value not greater than 40 PHN. If the value obtained is within 5 % of the assigned value, the instrument shall be consid ered to be in calibration. 16. Procedure 16.1 Unless otherwise specified, make the hardness deter mination at 73.5 3.5F (23 2C) and 50 5 % relative humidity, after holding the specimens under these conditions for not less than 24 h. 16.2 Rigidly attach the specimens to the instrument stage such that the surface to be measured is normal to the direction of indentation (Note 3). 16.3 With, a 1.0-kg load on the indenter, carefully bring the indenter into contact with the specimen surface, apply the full load, and start the timer. 16.4 At the end of 60 s, while still under full load, rapidly measure the diameter of the circular impression with the filar eyepiece of the microscope (Note 6). It is very important that the diameter measurements be made rapidly so that the time the indenter is in contact with the specimen is closely controlled.4 4 A hardness tester meeting the apparatus requirements of this method is the Head Indentation Hardness Tester, available from the United States Testing Co., IS Park Ave., Hoboken, NJ 07030. 16.5 From the measurements obtained in 16.4, the infor mation given in 14.2, and the measured film thickness at the place of indentation, calculate the depth of indenter penetra tion. If the depth of penetration exceeds three fourths of the coating thickness, the results may be influenced by substrate proximity. Therefore, for maximum accuracy it may be desirable to prepare thicker specimens and repeat the test. 16.6 Repeat the procedure in 16.3 and 16.4 until a total of at least five impressions have been made at widely spaced locations on the specimen. 17. Calculation 17.1 Calculate the mean indentation diameter in filar unils.- 17.2 Convert this mean indentation diameter to millimetres using the appropriate factor determined in 15.2. 17.3 Calculate the PHN as follows: - PHN = 1.27jd2 where: d = mean indentation diameter, mm. 18. Report 18.1 Report the following information: 18.1.1 Mean and range of PHN values obtained for each specimen, stating the number of indentations made, 18.1.2 Mean film thickness of the specimen, based on measurements made near the points of indentation'; 18.1.3 Specimen preparation and conditioning techniques used, and 18.1.4 Mean and. range of PHN values of the replicate pqnejs. 19. Precision 19.1 On the basis ofan interlaboratory test of this method in which operators in four laboratories tested seven coated panels having a broad range of hardness, the within-laboratory coefficient of variation was found to be 6 % with 28 degrees of freedom and the between-laboratories coefficient 12 % with 18 degress of freedom. Based upon these coeffi cients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 19.1.1 Repeatability--Two results, each themean ofthree determinations on a specimen, obtained by the same oper ator should be considered suspect if they differ by more than 18 % of their mean value. ` 19.1.2 Reproducibility--Two results, each the mean of three determinations on a specimen, obtained by operators in different laboratories should be considered suspect if they differ by more than 36 % of their mean value. 20. Keywords 20.1 hardness (indentation); hardness (Pfund); Knoop hardness tester; Pfiind hardness tester The American Society tor Testing and Materials takes no position respecting the validity ofanypatent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly adVlsed that determination ot the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility/., 9 -, ' - ... ,f. , Mi ,. ........................ '] ,-t * This standard Is subject to revision atany time by the responsible technical coritmittee arid must betevlawad every five years and ifnotrevlsedi either reapproved or withdrawn; Yourcomments are Invited either forrevision ofthis Standard or for additionalstandards and should ha addressed to ASTM Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee, which you may attend. It you feel thet your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Baca St., Philadelphia, PA 19103. 177 DUP050297360 <1 Designation: D 1475 - 90 Standard Test Method For Density of Paint, Varnish, Lacquer, and Related Products1 This standard is issued under the fixed designation D 1475; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This method has been approvedfor use by agencies afthe Department.ofDefense to replace Method 4184.1 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. 1. Scope 1.1 This test method covers the measurement of density ofpaints, varnishes, lacquers, and components thereof, other (25C) or at anagreed-upon temperature is then determined and density of the contents calculated in terms of grams per millilitre, or pounds per gallon at the specified temperature. than pigments, when in fluid form. 1.2 For higher precision when working with nonpigmented materials (drying oils, varnishes, resins and related materials). Test Method D 1963 can be used to determine specific gravity and, thence, density. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility of whoever uses this standard ta consult and establish appro priate safety and health practices and determine the applica 5. Significance and Use 5.1 Density is weight per unit volume. It is a key property in the identification, characterization, and quality control of a wide range of materials. Density measurements in terms of weight per-gallon are commonly used to check paint quality. If the density is not within specification, there is a go<xi chance that there was a mischarge or other serious problem. 5.2 This test method is suitable for the determination of N67' pycnom. usual lat triple-be. provide precisior 7.5 J reasons bility ofregulatory limitations prior to use. density of paint and related products and components when 2. Referenced Document in liquid form. It is particularly applicable when the fluid has too high a viscosity or when a component is too volatile for 3 8. Call) 8.1 r 2A ASTMStandard: D1963 Test Method for Specific Gravity of Drying Oils, Varnishes, Resins and Related Materials at 25/25C2 D4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter3 4 E 380 Practice for Use of the International System of Units (SI) (the Modernized Metrifc System)4 density balance determination.. 5.3 This test method provides for the maximum, accuracy required for hiding power determinations. It is-equally suitable for work in which less accuracy is required, by ignoring the directions for recalibration and consideration of temperature differentials, and using the container as a "weight-per-gallon" cup. 5.4 Automatic equipment for measuring density is aval- fled ten 8.1.1 weight, cleaner contains imum a< the difft exceed ( 3. Terminology 3.1 Definitions: 3.1.1 density--the mass (weight in vacuuip) of a unit volume of the liquid at any given temperature. In this method, it is expressed as the weight in grsuns per millilitre* oras the weight in pounds avoirdupois ofone U. SI gallon, of the liquid at the specified temperature; in the absence of other temperature specification, 25CJis assumed. I" 3.1.2 specific gravity--the ratio of the mass bf,(a unit volume of a material at a stated temperature to the mass of the same volume of distilled,water at the same temperature. 4. Summary of Test Method 4.1 The accurately known absolute density of distilled water at various temperatures (Table 1) is used to> calibrate the volume of a container. The weight of the paint liquid contents of the same container at the standard temperature able (see Test Method D 4052) from several manufacturers; Such, apparatus has been used for resins and latices as well as for oils and solvents. Before such equipment is used for 9 given product, results must be checked very careM|r Particularly with paints and resins, there are possibilities cl gumfning, fouling, and other interferences with operation.^ ( .Interferences .c 6.1 Highly viscous materials may entrap air andgS erroneous low density values. , rqsp ., 6.2 Paint liquids may be trapped in the ground glass^f metal joints of the pieces of apparatus, and give erroneoift high density values. tmoJ-l 7. Apparatus 7.1 Pycnometer--Any type, or weight-per-gallon (1 having a capacity of from 20 to 100 mL may be.usedljl on the c< Record 1 8.1.1.; corrosiv cause se In mak: care. In if exposi amounts clothing cleaning organic c supplier's tion. Ott effective. 8.1.2 F at a temj container provided that it may be filled readily with a viscous 1. remove e> adjusted to exact volume, and covered to exclude Ioss| }>y wiping 1 This test method is under the jurisdiction of ASTM Committee EM on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO! .24 on Physical Properties of Liquid Paints and Paint Materials. volatile matter. 7.2 thermometers, graduated in 0.TC, such as are i bubbles ir 8.1.3 B Current edition approved Oct. 26, 1990. Published December IggO. Originally plied with glass pycnometers., temperatu published as D 1475 - 57 T. Last previous edition D 7475 - 85. 2 Annual Book ofASTM Standards, Vol 06.03. ' !. Ilf: 5 Annual Book ofASTM Standards, Vol 05.03, 4 Annual Book ofASTM Standards, Vol 14.02. 7.3 Constant-Temperature Path, held at 25 0.1'G-1 desirable. 7.4 Laboratory Analytical Balance. 178 DUP050297361 letermined f grams per mperature. ey property y control of in terms of tint quality. : is a good us problem, mutation of ments when he fluid has /olatile for a im accuracy is-equally equired, by iideration of tainer as a sity is avail.mifacturers. :es as well as s used for a y carefully, ssibilities of iperation. sr and give und glass of e erroneous. --gallon cup, lay be used, iscous liquid, elude loss of h as are sup- 5 ore >s D 1475 TABLE 1 C 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 Absolute Density of Water, g/mL Density 0.999127 0.998971 0.998772 0.998623 0.998433 0.998231 0.998020 0.997798 0.997566 0.997324 0.997072 0.996811 0.996540 0.996260 0.995972 0.995684 N89' I--The usual weight-per-gallon cup and similar specialized pycnometers may have filled weights that exceed the capacity of the usual laboratory analytical balance. In such cases, use of a hanging pan, tnple-beam balance, with scales graduated to 0.01 g has been found to provide results the mean of which was consistent with the overall precision and accuracy ofthe method. 7.5 Desiccator and Desiccated Balance, or a room of reasonably constant temperature and humidity are desirable. g. Calibration of Pycnometer or Cup 8.1 Determine the volume of the container at the speci fied temperature by employing the following steps: 8.1.1 Clean and dry the container and bring it to constant weight Chromic acid (see 8.1.1.1) or other effective glass cleaner and nonresidual solvents may be used with glass containers and solvents with metal containers. For max imum accuracy, continue rinsing, drying, and weighing until the difference between two successive weighings does not exceed 0.001 % of the weight of the container. Fingerprints on the container will change the weight and must be avoided. Record the weight, M, in grains. 8.1.1.1 Precaution--Chromic acid cleaning solution is corrosive to skin, eyes and mucous membranes and can cause severe bums. Avoid contact with eyes, skin or clothing. In making dilute solution, always add acid to water with care. In case of contact, flush skin with water, using ashower ifexposure is severe. Flush eyes for 15 minutes with copious amounts of water. Immediately call a physician. Remove clothing immediately and wash before reuse. Chromic acid cleaning solution is a strong oxidizer. Avoid contact with organic or reducing substances as a fire could results. See supplier's Material Safety Data Sheet for further informa tion. Other cleaners are much safer and may be equally effective. 8.1.2 Fill the container with freshly boiled distilled water at a temperature somewhat below that specified. Cap the container, leaving the overflow orifice open. Immediately remove excess overflowed water or water held in depressions ty wiping dry with absorbent material. Avoid occluding air bubbles in the container. 8.1.3 Bring the container and contents to the specified temperature using the constant-temperature bath or room if necessary. This will cause further slight flow of water from the overflow orifice due to the expansion of the water with the rise of the temperature. 8.1.4 Remove the excess overflow by wiping carefully with absorbent material, avoiding wicking of water out of orifice, and immediately cap the overflow tube where such has been provided. Dry the outside of the container, if necessary, by wiping with absorbent material. Do not re move overflow that occurs subsequent to the first wiping after attainment of the desired temperature (Note 2). Imme diately weigh the filled container to the nearest 0.001 % ofits weight (Note 3). Record this weight, N, in grams. N:;' 2--Handling the container with bare hands will increase the temperature and cause more overflow from the overflow orifice, and will also leave fingerprints; hence, handling only with tongs and with hands protected by clean, dry, absorbent material is recommended. N<=' 3--Immediate and rapid weighing of the filled container is recommended here to minimize loss of weight due to evaporation ofthe water through orifices, and from overflow subsequent to the first wiping after attainment oftemperature where this overflow is not retained by a cap. 8.1.5 Calculate the container volume as follows: V = (N -- M)/p where: V = volume of container, mL, N = weight of container and water, g (7,1.4), M = weight of dry container, g (7.1.1), and p = absolute density of water at specified temperature, g/mL (see Table 1). 8.1.6 Obtain the mean of at least three determinations. 9. Procedure 9.1 Repeat the steps in Section 8, substituting the sample for the distilled water and a suitable nonresidual solvent for the acetone or alcohol (see 8.1.2 and Note 4). Record the weight ofthe filled container, W, and the weight ofthe empty container, w, in grams. N<=' 4--Trapping of paint liquids in ground glass or metal joints is likely to result in high values of density that appear to increase with the viscosity and density of the material; such errors should be minimized by firm seating of the joints. N>?' 5--Trapping ofair bubbles will result in low values for density. The tendency to trap air increases with increasing viscosity. Specimens should not be tested if they contain bubbles or foam. Slow stirring, standing, or the application of a vacuum may remove bubbles. If these do not work, a dilution may be necessary (see Appendix X1). 9.2 Calculate the density in grams per millilitre as follows: Dm = (W-w)/V where: Dm - density, g/mL. 9.3 Calculate the density in pounds per gallon as follows: D = (W -- w)K/V where: D = density, lb/gal, K = 8.3454 (Note 6), and V = volume of container, mL (see 8.1.6). 179 DUP050297362 NOTE 6--The factor K, 8.3454, is calculated from volume-weight relationship as follows: The results were analyzed statistically in accordance with Practice E 180. The within-laboratory coefficient of variation 8.345404 = [(2.54)3<* X (231.00)*]/(453.59237)c was found to be 0.20 % relative with 25 degrees of freedom and the between-laboratoiy coefficient of variation was " (2.54)3 is the conversion factor for millilitres to cubic inches. h 231.00 is the conversion factor for cubic inches to gallons. *'453.59237 is the conversion factor for grams to pounds. 0.61 % relative with 20 degrees of freedom. Based on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 10. Report 11.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator on 10.1 In reporting the density, state the test temperature to the nearest 0.TC, the units, and the value calculated to the third place to the right of the decimal point (for example, D -- x.xxx lb/gal at 25C); state the mean, the range, and the number of replicate determinations. 11. Precision and Bias 11.1 The precision estimates are based on an interiaboratory study in which one operator in each of six different laboratories analyzed in duplicate on two different days five samples of paint ranging in density from 8.5 to 12.5 lbs/gl. different days should be considered suspect if they differ by more than 0.6 % relative. 11.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 1.8 % relative. 11.2 No data on bias has been generated for this test method. 12. Keywords 12.1. density; pycnometer; weight per gallon; weight per gallon cup 1. & 1.1 comi finis! i.: atior. addr the i appr APPENDIX apph haza (Nonmandatory Information) XI. Diluting of a Material to Improve Air Release Nc D 13( Xl.l To reduce viscosity and improve air release, a known weight ofa material that traps air may be diluted with a known weight of a solvent or another diluent of known density. After careful blending to achieve homogeneity and release air, the density ofthe diluted material is measured by the technique described in this test method. The following equation may be used to calculate the density of the original material: D ^ + WA WA Ail Att where: Da = density of original material, An = density diluted measured in test, A12 = density diluent, Wa -- original weight, and Wd = diluent weight. The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must boreviewed every live years and it notrevised, eitherreapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 79T03. 2. R 2.: D D D 3. S 3. desc havi that 4. S 4. dure apph pear; the t man blistt ii> 'life i T Relate D01.2 Cu' Publis: XA 3A .... ................---, 180 _______ .___:----------------------- DU P050297363 lance with if variation of freedom iation was :d on these for judging ; level: lean of duperator on :y differ by s mean of in different y differ by >r this test weight per dll|M Designation: D 1540 - 82 (Reapproved 1987)ei Standard Practice for Effect of Chemical Agents on Organic Finishes Used in the Transportation Industry1 This standard is issued under the fixed designation D 1540; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates ihe year of last reapprovai. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. ``N@A' --Paragraph 1.2 was changed editorially and footnote 4 added editorially in May 1987. 1. Scope 1.1 This practice covers determination of the effect of commonly encountered chemical agents on applied organic finishes used in the transportation industry. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use.-It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine die applicability of regulatory limitations prior to use. Specific hazard statements are given in Note 3. NBC' I--This practice is a companion standard to Test Method 0 1308. 2. Referenced Documents 2.1 ASTM Standards: 6^ D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D925 Test Methods for Rubber Property--Staining of Surfaces (Contact, Migration, and Diffusion)3 D1308 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes2 3. Summary of Test Method 3.1 The test surface is subjected to test by contact, as described in 7.2, 7.3, or 7.4, with an agent suspected of having a deleterious effect, under conditions appropriate to that agent. 4. Significance and Use 4.1 This practice is designed'to provide a working proce dure for the examination of the effect of chemical agents on applied transportation finishes. Any change in surface ap pearance or condition reflects an objectionable tendency of the finish to be affected by the agent used. The change is manifested by softening, swelling, discoloration, loss of gloss, blistering, loss of adhesion, or other special phenomena. 1 This practice is under the jurisdiction ofASTM Committee D-l on Paint and dieted Coatings and Materials and is the direct responsibility of Subcommittee 001.27 on Accelerated Tests for Protective Coatings. Current edition approved Sept 1, 1982. Published November 1982. Originally Published as D1540 - 58 T. Last previous edition D 1540 - 61 (1973). 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 09.01. 5. Test Panels 5.1 Steel Panels--Steel panels as described in Methods D609. 5.2 Other test surfaces may be agreed upon between the purchaser and the seller of the finish being tested. 6. Chemical Agents 6.1 The choice of the agent shall be governed by ultimate coating use and by agreement between the purchaser and the seller ofthe finish being tested. The following staining agents are listed as being of general interest. 6.1.1 Glycol based antifreeze up to 100 volume, %. 6.1.2 Add, alkali, and salt solutions, 6.1.3 Soap and synthetic detergent solutions, ' 6.1.4 Lubricating oils and greases, 6.1.5 Polish abrasives, creams, waxes, 6.1.6 Road oils and tars; seam sealers, 6.1.7 Rubber or other elastomers; plastics, tapes, 6.1.8 Gasolines, 6.1.9 Water, 6.1.10 Hydraulic fluids, 6.1.11 Alcohol windshield washing compounds, and 6.1.12 Others. 7. Procedure 7.1 Panel Preparation--Carry out spot and direct applica tion tests on the fabricated article coated with the finishing system under evaluation, if sufficient plane surface is avail able. Otherwise, select panels in accordance with 5.1. Apply the finishing system in accordance with the method and schedule prescribed by the purchaser. Age the finished film to suit the exposure conditions, as agreed between the purchaser and the seller of the film-forming material. 7.2 Spot Testfor Liquid Agents--Conduct the test at 73 3.5*F (23 2"C) and 50 5 % relative humidity. Place a small portion of the staining agent on a horizontal test surface, making several spots approximately 1 in. (25 mm) in diameter. After the time agreed upon has elapsed, such as 4, 8,24, and 72 h, wipe off a spot, and examine it immediately for visual and physical evidence of the effects listed ip Section 4. Polish die test surface lightly with any suitable liquid car cleaner, and evaluate the surface in accordance with agreement on the basis of removability. Expose the test surface to sunlight for at least 8 h, or to strong ultraviolet light (Note 2) at 150T (65C) or less as agreed upon, for 1 h. Evaluate the surface on the basis of either disappearance of defects or development of defects not previously visible. 181 DUP050297364 # D 1540 Prepare surfaces for water spotting tests by exposing them to an RS ultraviolet lamp for 6 h, and then polishing. Then proceed as follows: apply water drops, heat in an oven at 150F for 15 min, and then lightly polish. Any variations in the procedure shall be as agreed upon between the purchaser and the seller of the film-forming material. NDE' 2--The RS sunlamp manufactured by the General Electric Co. is recommended for this test. Other ultraviolet light sources are acceptable if agreed upon by the purchaser and seller, and if the appropriate exposure equivalent is known and used. 7.3 Contact Test for Solids--The materials listed in 6.1.7 may produce a deterioration of the appearance in several of the ways listed in Section 4, but must be held in close contact with the surface. Frequently the agent may cause an effect only when heated, therefore, they should be heated for this test. Test finishes with rubber as a staining agent, in accordance with Test Methods D 925. Plastics may be hdld in contact with the finish, and tested as described in 7.2. 7.4 Gasoline (Caution; Note 3)--To determine the' staining effect of gasoline, place some in a buret Allow th^ gasoline to fall 4 in. (100 mm) onto the test surface placea below and at an angle of 20 from the horizontal. The dropping rate should be about 10 drops per minute. Place an RS sunlamp (Note 2) 15 in. (380 mm) from the test surface so that its rays shine at 90 to the surface. Continue the test until 200 mL of gasoline have been dropped during 3 V2 h. NFG' 3: Caution--This test should be run where there is adequate ventilation,'and'provision should be made for draining the drippings into a safety can. Other precautions against fire should be observed. 7.5 In evaluating the results, the 0 to 10 scale prescribed in ASTM STP 50(f should be used. 8. Report 8.1 Report the following information: 8.1.1 The system and the test method employed. Test conditions are an important factor in the results obtained, and therefore, should be defined in the report 8.1.2 The type and appearance of the effect obtained, if any, (see Section 4). It is customary to record stain-free contact time as a basis of comparison. Where agreed, the effect of the agent may alsobe evaluated by the use of a color difference meter spectrophotometer, glossmeter, hardness instrument or other applicable apparatus. * Paint Testing Manual, ASTM STP 500, ASTM, 1972. The American Society lor Testing and Materials takes no position respecting the validity ofany patent rights assertedIn connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of.such rights, areentirely their own responsibility. This standard Is sub/ect to revision at any time by the responsible technicalcommittee and must be reviewed every five years and Ifnotrevised, either reapproved or withdrawn. Yourcomments are invited either for revision of this standard or tar additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 1910$.,, <1! , lU!.' I J * lit ,u-'. X 1T and R mittee Cui publish 182 DUP050297365 test suifa^ nue the test ring 3Vi h. re is adequ^ 3 observed, described in >loyed. Test ts obtained, obtained, if d stain-free agreed, the se of a color it , hardness f Designation: D 1542 - 60 (Reapproved 1988)61 Standard Test Method for Qualitative Detection of Rosin in Varnishes1 This standard is issued under the fixed designation D 1542| the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Depanmem ofDefense to replace Method 5031, 5032 of Federal Test StandardNo. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. <> HIJ' --Editorial changes were made throughout, including the title, in May 1988. 1. Scope 1.1 This test method covers procedures for the qualitative detection of rosin in varnishes by the Lieberman-Storch Test, and the Halphen-Hicks Test. The rosin may be present as either free rosin (abietic acid), esterified rosin, or as metal salts. ' 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Apparatus 2.1 Test Tubes, 2.5 by 15 cm. 2.2 Filter Funnel, 75 mm in diameter. 2.3 Porcelain Spot Plate. 3. Reagents 3.1 Acetic Anhydride. 3.2 Bromine Reagent--Dissolve 1 part by volume of bromine in 4 parts by volume of carbon tetrachloride (CCL4). 3.3 Phenol Reagent--Dissolve 1 part by volume ofphenol in 2 parts by volume of carbon tetrachloride (CCL4). 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DOt.33 on Varnish and Resins, Including Shellac. Current edition approved Sept. 19,1960. Published November 1960. Originally published as D 1542 - 58 T. Last previous edition D 1542 - 58. 3.4 Sulfuric Acid Reagent--Add 35.7 mL of concentrated sulfuric acid (H2S04, sp gr 1.84) slowly to 34.7 mL of water, and cool to room temperature. Store in a glass-stoppered bottle. - 4. Procedure 4.1 Lieberman-Storch Test--Place 0.1 to 0.2 g of the sample in a test tube, and add 15 mL of acetic anhydride. Heat gently until the specimen is dissolved or dispersed. Cool and filter with an ashless rapid filter paper, into a clean test tube. Place a few drops of the clear solution in a depression of the spot plate, and add one drop of sulfuric acid reagent, so that the add will mix slowly with the filtrate. If rosin is present, a fugitive violet color develops immediately. A pink or brown coloration should be ignored. A control spedmen containing rosin should be run simultaneously. 4.2 Halphen-Hicks Test--Dissolve a small quantity of the sample in 1 to 2 mL ofthe phenol reagent Pour the solution into a cavity of the spot plate until it just fills the depression. A portion of the solution will spread out on the flat part of the plate a short distance beyond the rim of the cavity, unless too much of the carbon tetrachloride has been lost by evaporation, when a drop or two more should be added to produce the spreading effect referred to. Immediately in an adjacent cavity, place 1 mL or more of the bromine reagent, so that the bromine vapors evolved will contact the surface of the solution in the other cavity. Sometimes it is necessary to blow a gentle current of air in the proper direction to accomplish this satisfactorily, or both cavities may be cov ered by a watch glass of suitable size. The development of a fugitive violet coloration, best observed upon a flat portion of the test plate, indicates the presence of rosin. Tha American Society tor Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and tha risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Yourcomments ate Invitedeither forrevision ol this standard orforadditional standards and should be addressed to ASTM Headquarters. Your comments will receive caretul consideration at s meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 183 DUP0502 97366 Last ASTM Designation: D 1543 - 86 Standard Test Method for Color Performance of White Architectural Enamels This test method describes a laboratory procedure for evaluating the color permanence of white architectural enamels. Formerly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials. This test method was discontinued in 1992. \ l I f | 2. R 2.1 D I ': < 3. A) 3.1 the c dure color 3.2 about descri 3.3 stand; have 3.3. 3.3. signifi and si 3.3. 'Thi Coatings Properti, Currc Publishe 2 Ann 3 Ann 184 DUP0502 97367 Designation: D 1544 - 80 (Reapproved 1989)61 Standard Test Method for Color of Transparent Liquids (Gardner Color Scale)1 This standard is issued under the fixed designation D 1544; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies of the Department ofDefense to replace Method 4248 of Federal Test Method Standardbio. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. " NKL' --Editorial changes were made throughout in April 1989. 1. Scope 1.1 This test method covers the measurement of the color of transparent liquids by means of comparison with arbi trarily numbered glass standards. It applies to drying oils, varnishes, fatty acids, polymerized fatty acids, and resjn solutions. Its application to other materials has not been tested. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport io address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method2 E 308 Method for Computing the Colors of Objects by Using the CIE System3 3. Apparatus 3.1 Glass Standards, 18, numbered separately, and having the color characteristics given in Table 1. A suitable proce dure for their calibration is contained in Appendix Al. The color shall be produced by the glass components only. 3.2 Glass Tubes, clear, 10.65 mm in inside diameter and about 114 mm in outside length. (Viscosity tubes, as described in Test Method D 1545, are satisfactory.) 3.3 Suitable apparatus for comparing sample and standard. The apparatus may be of any design, but should have the following characteristics: 3.3.1 Illumination--CIE Illuminant C. 3.3.2 Surrounding Field--The field should not differ significantly in brightness from the samples and standards and should be essentially achromatic. 3.3.3 Field of View--The specimen and one or more TABLE 1 Color Specifications of Reference Standards Gardner Color Standard Number Chromaticity Coordinates'1 Xy Luminous Transmittance Transmittance Tolerance, Y, % 1 0.3177 0.3303 2 0.3233 0.3352 3 0.3329 0.3452 4 0.3437 0.3644 5 0.3558 0.3840 6 0.3767 0.4061 7 0.4044 0.4352 8 0.4207 0.4495 9 0.4343 0.4640 10 0.4503 0.4760 11 0.4842 0.4818 12 0.5077 0.4638 13 0.5392 0.4458 14 0.5646 0.4270 15 0.5857 0.4089 16 0.6047 0.3921 17 0.6290 0.3701 18 0.6477 0.3521 80 7 79 7 76 6 75 5 74 4 71 4 67 4 64 4 61 4 57 4 45 4 36 5 30 6 22 6 16 2 11 1 61 41 * A duplicate standard shall have chromaticity coordinates that differ from the reference standard by no more than one third of the difference in x or y between adjacent reference standards. In any one set, no two standards shall be closer together than two thirds of the difference in x or y between corresponding reference standards. standards should subtend a visual angle of about 2 deg and be in the field of view simultaneously. 3.3.4 Separation of Standard and Specimen--There should be a perceptible separation between specimen and standard, but this should be as small as is mechanically possible. 4. Procedure 4.1 Fill a glass tube with the material under test. If the material is perceptibly cloudy, first filter it 4.2 Compare with glass standards, determining which standard most closely matches the specimen in brightness and saturation. Ignore hue differences. 'This method is under the jurisdiction ofCommittee D-l on Paint and Related Coalings and is the direct responsibility of Subcommittee DO 1.26 on Optical Properties. Current edition approved March 10, 1980. Published May 1980. Originally Published as D 1544-58 T. Last previous edition D 3544 - 68 (1974). 1 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 3 Annual Book ofASTM Standards, Vol 14.02. 5. Report 5.1 Report the color as the number of the standard most closely matching the specimen. If more precise measure ments are needed, report as either matching a standard or lighter or darker. Thus, between colors 5 and 6, the steps will be 5, 5+, 6--, and 6. 1$S DUP050297368 D 1544 6. Precision and Bias 6.1 On the basis of a study in which one observer at each of 80 laboratories made duplicate determinations on four samples, the "between" and "within" standard deviations were found to be 0.5 and 0.1 color number, respectively. Based on these standard deviations, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level. 6.2 Repeatability--Two results obtained by a single oper ator should be considered suspect if they differ by more than two thirds of a color number. 6.3 Reproducibility--Two results, each of the mean of duplicate measurements, made by operators in different laboratories should be considered suspect if they differ by more than four thirds of a color number. NMN' 1--If desired, liquid standards matching the colors given in Table 1, in glass tubes similar to the sample tubes may be used. These may be filled with potassium chloroplatinate for the light colors and solutions of ferric chloride and cobalt chloride in hydrochloric acid for the darker colors. The specifications and approximate composition of these solutions are given in Test Method D 1544 - 58 T.4 Many Glass Standards in current use do not conform to the values of Table 1. NMN' 2--The precision data were obtained using an instrument in which two standards are viewed simultaneously. There are other instruments available for color matching which would be expected to give similar results, but the statement above applies only to the instrument checked. 1 s ! j 1 I I I-------------------------------------------------------------------------------------- 4 See 1961 Book ofASTM Standards, Part 8. 1 | APPENDIX (Nonmandatory. Information) XI. CALIBRATION OF GLASS REFERENCE STANDARDS Xl.l Select a dual beam spectrophotometer with a suffi ciently small light beam at the sample position so that all rays will pass through the standards to be calibrated. Alter natively equip the spectrophotometer with a condensing lens to accomplish this purpose. X1.2 Place the standards in turn in the sample position of the spectrophotometer. If the comparator is provided with a separate green filter in front of the light source, place this filter in the reference beam ofthe dual beam spectrophotometer during calibration of each standard. X1.3 Obtain spectral transmittance data for each glass reference standard by following Method E 308. X1.4 From the spectral transmittance data for each reference standard calculate the CIE tristimulus values, X, Y, Z, and the chromaticity coordinates, x, y, for CIE Illuminant C (see Method E 308). 1 ` I ' ! S The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must ba reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments areinvited either tor revision of this standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you fee! that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1918 Ftace St., Philadelphia, PA 19103. f ! | I f l. vis art atl ad thi ap ap 2. of ab is art vis 3. pa as be in fO! i! Th i o.; j the j i i 1 and mit 186 DUP050297369 Designation: D 154589 ilors given i,, e used. These ht colors and iloric acid fQ( imposition 0. ` Many Glass Table 1. nstrument in te are other e expected to only to the trophotomeach glass each referes, X, Y, Z, luminant C Standard Test Method for Viscosity of Transparent Liquids by Bubble Time Method1 This standard is issued under the fixed designation D 1545; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 4271 of Federal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This test method covers the determination of the viscosity in bubble seconds by timing. The bubble seconds are approximately equal to stokes for most liquids. 1.2 The test method is applicable to transparent liquids that are free from crystalline or gel particles. 1.3 This standard may involve hazardous materials, operdiions, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is ihe responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. I, Terminology 2.1 Definition: 2.1.1 viscosity--the resistance experienced by one portion of a liquid moving over another portion of the liquid. The absolute unit of viscosity in the cgs system is the poise which is expressed as dyne-seconds per square centimetre. Stokes are equal to poises divided by density. The absolute SI viscosity unit is the pascal-second. 3. Apparatus 3.1 Constant-Temperature Bath--Any suitable bath ca pable of maintaining temperature at 25 0.1C with water as the bath medium. 3.2 Standard Viscosity Tubes,2 of clear glass and with flat bottoms, 10.65 0.025 mm in inside diameter, 114 1 mm in outside length. Plainly legible lines shall be located as follows (Note 1): 27 0.5 mm 100 0.5 mm 108 0.5 mm The distance between the first and second lines shall be 73 0.5 mm. NOP' 1--All distances shall be measured from the outside bottom of the tube. 3.3 Reference Standards--A series of standard viscosity 1 This test method is under die jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.33 on Polymers and Resins. Current edition approved Oct. 27, 1989. Published December 1989. Originally Published as D 1545 - 58 T. Last previous edition D 1545 - 76(1989)". 'Empty standard viscosity tubes are available from the R. P. Cargille Laboratories, Inc., 33 Village Park Rd.. Cedar Grove, NJ, or Byk-Gardner Inc., Gartner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. tubes (3.2) filled with transparent liquids having predeter mined viscosities in stokes and bubble seconds and spaced in logarithmically even increments of about 26 % (log 1.260 = 0.100), as listed in Table 1. The standards shall be marked alphabetically or numerically as shown in Table 1 without reference to stokes or bubble time (Note 2). Also listed in Table 1, for general and historical reference only, is the long established series of Gardner-Holdt letter standards, in tubes that do not have the three lines and are shorter than the standard viscosity tubes described in 3.2. NQR' 2--For convenience, the reference standards can be divided in three series: light series, 15 tubes marked 0.22 to 8.0; heavy series, 14 tubes marked 10 to 200; and very heavy series, 7 tubes, marked 250 to 1000. 3.4 Timing Device--Stopwatch or electric stop clock capable of being read to a precision of 0.1 s. 3.5 Tube Racks, capable of inverting one or more viscosity tubes 180 to within 1 of a vertical position while rack and tubes are immersed in the constant temperature bath. 3.6 Viscosity Tube Corks, No. 2 short. 4. Procedure 4.1 Fill a standard viscosity tube with the material to be tested to approximately level with the 108-mm line. 4.2 Transfer the tube to a constant 25C temperature bath with the cork loosely inserted. Hold at this temperature for 10 min. NST' 3--Adequate control of the temperature bath is essential. A variation of 0.1C in the temperature of the bath will cause a 1 % variation in the timed bubble travel. 4.3 At the end of 10 min adjust the level of the liquid so that the bottom meniscus will be level with the 100-mm line. Insert the cork so that the bottom of the cork is on the level with the 108-mm line. This will ensure a bubble of suitable and uniform size, 4.4 Insert the tube in the rack and immerse in the 25C water bath. Allow the tube(s) to stand with cork down in the bath a minimum of 20 min before determining the viscosity. NUV' 4--For viscosities ofliquids that have a timed bubble travel of 4 s or less, more precise results can be obtained by comparison against reference standards having a predetermined viscosity or timed bubble travel. 4.5 To read, invert the tube quickly and determine the time required for the bubble to rise in seconds. When determining the time in seconds start the timing device when the top of the bubble becomes tangent to the 27-mm line on 187 DUP050297370 D 1545 TABLE 1 Recommended Numerical Standards tor Comparator Viscosity Tubes4 the tube. Stop the timing when the top of the bubble becomes tangent with the 100-mm line. This gives a 73-mm timed bubble travel. All timings shall be made with the tube in an exact vertical position. NWX' 5--Positioning ofthe tube in a vertical position is mandatory. A tube one radius off the vertical will give an error of approximately 10 % in the time of bubble travel. 5. Report 5.1 Report the following information: 5.1.1 The viscosity obtained by the timing method expressed as "bubble seconds" or "approximate stokes." NYZ' 6--The time in seconds or "bubble seconds" is an approxi mate measurement ofstokes when the bubble time method is applied to most raw materials and finished products encountered by the paint, varnish, and lacquer industries. This relationship does not hold for silicones or water dispersions of gums or similar materials. Viscosity results by this test method are influenced by non-Newtonian behavior aifd by surface tension. Other variations on bubble-tube viscometers are described in ASTM STP 500, Section 3.2.9.3 6. Precision and Bias 6.1 On the basis of an interlaboratory study4 of this test method in which ten laboratories tested liquids ranging in viscosity from 4.5 to 440 St, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 6.1.1 Two results obtained by the same operator should be considered suspect if they differ by more than 4.9 % relative. 6.1.2 Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 9.0 % relative. ! j | j I Gardner-Holdt letters. Stokes are shown in logarithmic progression. i aThe bubble time, in seconds, of the numerical tubes under 4 s was determined by a technique employing a movie camera. 0 For reference purposes only. Numbered tubes are no longer commercially available. 0 Above 2.65 the bubble seconds as measured by the kinematic method are i: approximately equivalent for most products. Below 2.65 this relationship does not hold. 3 Paint Testing Manual, ASTM STP }00, ASTM, 1972. 4 See Holt, K. E-, Proceedings, ASTM, Vol 57, 1957, pp. 297-300, and Official Digest, Federation of Societies for Paint Technology, Vol 30, May 1958, pp> f 540-543. 188 DUP050297371 e bubble a 73-mm the tube | 1 1 1 nandatory, roximately :thod exs." n approxi; applied to the paint, >t hold for . Viscosity n behavior >meters are this test mgjng in ihould be the 95 % yt should in 4.9% obtained jnsidered # D 1545 , The American Society for Testing and Materials takes noposition respecting the validity ofany patentrights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. ' This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are Invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. and Official .y 1958, PP- 1 . . -'r . ' ; :* > .t*v t ..... '1 189 DUP050297372 /(DIM Designation: D 1546 - 62 (Reapproved 1987) Standard Method for Performance Tests of Clear Floor Sealers1 This standard is issued under the fixed designation D 1546; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapptovaL A superscript epsilon () indicates an editorial change since the last revision or reapprovai. 1. Scope 1.1 This method covers the testing ofclear floor sealers for appearance of finish, treatment of worn areas, the applica tion of finishing materials such as varnish, liquid or paste waxes either solvent or emulsion type, and resistance to ink staining. NOTE l--The resistance of the sealer to other reagents may be determined by this procedure when agreed upon by the purchaser and the seiler. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safetyproblems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 U.S. Federal Specifications: P-W-155 Solvent Wax2 P-W-158 Emulsion Wax2 TT-I-563 Blue-Black Ink2 TT-V-71-f Varnish2 3. Apparatus 3.1 Maple Panels--First grade maple flooring 2xh by 12 in. (64 by 305 mm). 3.2 Sandpaper--No 0 and 00 garnet paper. 3.3 Cheesecloth. 3.4 Blotting Paper. 4. Materials 4.1 Blue-Black Ink, (Federal Specification TT-I-563). 4.2 Varnish, (Federal Specification TT-V-71-f). 4.3 Solvent Wax, (Federal Specification P-W-158). 1 This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D 01.33 on Varnish and Resins, including Shellac. Current edition approved Sept. 28,1962. Published November 1962. Originally published as D 1546 - 58 T. Last previous edition D 1546 - 58. 2 Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 4.4 Emulsion Wax, (Federal Specification P-W-155). 5. Panel Preparation 5.1 Sand the five maple panels with No. 00 garnet paper until the surface is flat and smooth. Remove the excess sanding dust with a clean dry cloth. 5.2 Apply a liberal coat of sealer to the panels using a pad of clean cheesecloth. Note fluidity and ease of application. Allow the sealer to set 15 min for absorption into the wood. Wipe off the excess sealer using a pad of cheesecloth (note , whether the excess sealer removed in this manner can be wiped readily and cleanly from the surface). The surface shall be free of all excess sealer. Allow the panels to dry 24 h at a temperature between 70 and 90T (21.1 and 32.2'C). 5.3 Apply a second coat of sealer following the procedure described in 5.2. N[\' 2--Other methods of application and panel preparation may be used when agreed upon by the purchaser and the seller. 6. Procedure 6.1 Appearance ofFinish--Examine the panel, treated as described in Section 5, for the presence of surface film. Note whether the treated surface of the panel has a soft, even sheen and whether the grain of the wood is douded or obscured. 6.2 Resistance to Ink Stain--Place several drops of blueblack ink on the surface of a treated panel at various places and allow to remain for 3 min. Take up the ink with blotting paper and wipe the spots lightly with a damp cloth. Examine the surface for any indication of the presence of ink. 6.3 Treatment of Worn Spots--Simulate on a treated panel worn areas by rubbing the surface with No. 0 steel wool. Over these pands apply a thin coat of sealer. Burnish the worn areas with No. 00 steel wool immediately after application of the sealer. When dry, examine the treated areas to determine whether they blend with the surface ofthe panel without showing any signs of lap marks. 6.4 Application, of Finishing Materials--To a treated panel apply a finish coat of the varnish. To a second treated panel apply a coat of the solvent wax. To a third treated panel apply the emulsion wax. Note whether the properties ofthe finishing materials are adversely affected by the sealed surface or whether the finishing material adversely affects the sealed surface. 190 DUP0502 97373 5). t paper excess gapad ication. ; wood, ii (note can be ce shall 1 h at a icedure ion may ated as i. Note t, even ded or >f blue places dotting (amine reated ) steel amish after reated ofthe treated treated treated jperties : sealed acts the D 1546 The American Society for Testing andMaterials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility.' ' f This standard is subject to revision at any time by the responsible technical committee aridmust be reviewed every five years and itnot revised, either reapproved or withdrawn. Yourcomments are Invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical commHtae, which you may attend, if you fee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St.. Philadelphia, PA 19103. \ :l 191 DUP050297374 4 Designation: D 1639 - 90 Standard Test Method for Acid Value of Organic Coating Materials1 This standard is issued under the fixed designation O 1639; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<} indicates an editorial change since the last revision or reapprovaL This standardhas been approvedfor me bp agencies ofthe Department ofDefense to replaceMethods 5071.5072,5073 ofFederal Test MethodStandard No. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This test method covers the measurement of the free acidity present in the nonvolatile portion of varnishes, oils, certain resins, and paint vehicles, by the reaction with 4.2 This test method also provides a convenient method of process control for the manufacture of certain resins and paint vehicles designed to meet particular requirements of the buyer and the seller. standard alkali solution. 1.2 If carboxylic anhydrides are present, only one half of 5. Reagents and Solvents the reactive groups will be titrated and indicated by this test 5.1 Purity ofReagents--Reagent grade chemicals shall be method. used in all tests. Unless otherwise indicated, it is intended 1.3 This standard does not purport to address the safety that all reagents shall conform to the specifications of the problems associated with its use. It is the responsibility ofthe Committee on Analytical Reagents of the American Chem user of this standard to establish appropriate safety and ical Society, where such specifications are available.5 Other health practices and determine the applicability ofregulatory grades may be used, provided it is first ascertained that the limitations prior to use. reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 2. Referenced Documents 5.2 Phenolphthalein Indicator Solution (10 g/L)--Dis solve 1 g of phenolphthalein in 100 mL of methanol, 11 2.1 ASTM Standards: ethanol, or isopropranol. D 362 Specification for Industrial Grade Toluene12 D770 Specification for Isopropyl Alcohol2 D1259 Test Methods for Nonvolatile Content of Resin 5.3 Potassium Hydroxide, Methyl Alcohol (Methanol) Solution (1 mL = 5.6 mg KOH)--Dissolve 6.6 g of potas sium hydroxide (KOH) in 1 L of methyl alcohol. Standardize Solutions3 against National Institute of Standards and Technology D1644 Test Methods for Nonvolatile Content of standard potassium hydrogen phthalate Standard Reference Varnishes4 No. 84, using phenolphthalein as the indicator (5.2)1 Do not D1960 Test Method for Loss on Heating of Drying Oils2 adjust the concentration of the solution, but calculate the 3. Terminology 3.1 Definition: 3.1.1 acid value--the number of milligrams of potassium hydroxide (KOH) required to neutralize the alkali-reactive milligrams of KOH per litre of solution, K. (See Note.) NOTE l--At the discretion of the purchaser and the seller, an aqueous solution ofpotassium hydroxide of0.1 Nor 0.5 N may be used. N]^' 2--Potassium hydroxide, methyl alcohol (methanol) solution may be purchased from most major laboratory chemical supplier groups in 1 g of material under the conditions of test (see houses. This material should be standardized as just indicated. 6.4). 5.4 Neutral Solvent Mixture--Mix equal parts by volume 4. Significance and Use of isopropyl alcohol (isopropanol) (see Specification D 770) and industrial toluene (see Specification D 362). Neutralize 4.1 This test method is used to determine the free acidity the mixture using 0.1 N KOH solution (4.3) and phenoi- present in the nonvolatile portion of varnishes, oils, certain phthalein indicator solution (5.2) until the pink color persists resins, and paint vehicles by the reaction with a standard for 1 min. alkali solution. Use of this test method provides a means whereby the relativeapplicability ofthe varnish, oil, resin, or 6. Procedure paint vehicle to the particular end use may be estimated by the buyer and the seller. 6.1 Weigh or transfer into a 250-mL Erlenmeyer flask the specimen mass, S, prescribed in Table 1. 6.2 Add 100 mL of neutral solvent Mix until all material 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint is dissolved, warming if necessary. Cool to room tempera and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.33 on Polymers and Resins. Current edition approved Oct. 26,1990. Published December 1990. Originally published as D 1639-61. Last previous edition D 1639-89. 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vol 06.01. the American Chemical Society, see "Reagent Chemicals and Standards,' by Joseph Rosin, D. Van Nostnmd Co., Inc., New York, NY, and the "United States Pharmacopeia." 192 ture, pher KOI persi 6..' 6.` mine Met! metb 7. G 7.1 DUP050297375 method sins and uents of ; shall be intended is of the n Chem:-5 Other that the ; without L)--Dislethanol, 'ethanol) of potasndardize :hnoIogy Reference i. Do not ulate the >te.) seller, an iy be used. ) solution supplier volume , D770) jutralize phenol r persists TABLE 1 Specimen Size Expected Add Value Approximate Spedmen Mass, g ' 0 toS Over 5 to 15 Over 15 to 30 Over 30 to 100 Over 100 20 10 5 2.5 1 Accuracy of weighing, plus or mi nus, mg 50 50 50 1 1 about 77"F (25C), before titrating. Add 1 mL of Solphthalein indicator solution and titrate with the 0.12V fori solution (5.3) to the end point, which is a pink color Insisting for 30 s (F). j 3 Repeat with a second specimen. j 4 In the case of materials containing a solvent, deterthe nonvolatile content in accordance with Test SUods D 1259, D 1644, D 1960 or other applicable Method agreed upon between the purchaser and the seller. 7. calculation 7.1Calculate the acid value A as follows: where: V -- volume of KOH solution required for titration of the specimen, mL, K = weight of KOH per millilitre of KOH solution, g, S = specimen weight, g, and N - nonvolatile content of the material expressed as a decimal fraction. 7.2 Calculate the mean of the two runs. 8. Report 8.1 Report the acid value of the nonvolatile matter to the nearest decimal (0.1). 9. Precision 9.1 Because of the many types of material covered by this test method, the precision is not as good as might be ex pected of a quantitative analytical method. The following criteria should be used forjudging the acceptability of results: 9.1.1 Repeatability--Duplicate results obtained by the same operator should be considered suspect if they differ by more than 10 % of the mean acid value. 9.1.2 Reproducibility--Two results obtained by operators in different laboratories should be considered suspect if they differ by more than 20 % of the mean acid value. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity ot any such patent rights, and the risk of Infringement of suoh rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelptiia, PA 19103. i flask the material tempera- Am. Chemnot listed by ndards," W Jnited States 193 DUP050297376 i Designation: D 1640 - 83 (Reapproved 1989)^ 6.1.1 All one operat Standard Test Methods for Drying, Curing, or Film Formation of Organic Coatings at Apply the s examinatio hours of th Room Temperature1 6.1.2 Ap panels or agreed upo This standard is issued under the fixed designation D 1640; die number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This standard has been approvedJar use by agencies of the Depanmem of Defense. Consult the DoD Index of Specifications and Standards for the specific year ofissue which has been adopted by the Department ofDefense. glass plates that tend tc plates can 1 glass by gr water betw (1 N_`' --Editorial changes were made throughout in April 1989. 6.1.3 Tt blade havii dry film tl 1. Scope coatings or ingredient changes,'or both. This is significant in doctor blat ji .] 1 1.1 These test methods cover the determination of the various stages and rates of film formation in the drying or curing of organic coatings normally used under conditions of ambient room temperature. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish, appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. the development of organic coatings for various end uses and also for production quality controL 4. Coatings and Recommended Film Thicknesses 4.1 Whenever tests are to be performed on coatings not listed in Table 1, there should be a prior agreement between the purchaser and seller as to the substrate, film thickness, and application method for testing the specific coating involved. 5. Test Conditions apply the tional and applicatior conform t Methods : methods o 6.1.4 M proper filr comparatc D 1005. VI dry film tfc 2. Referenced Documents 5.1 Conduct all drying tests in a-well-ventilated room or after coati chamber, free from direct drafts (Note 1), dust, products of solids. 2.1 ASTM Standards: combustion, laboratory fumes and under diffused light (see D202 Methods of Sampling and Testing Untreated Paper 5.4). Make all measurements at a temperature of 23 2'C 7. Proced Used for Electrical Insulation2 and 50 5 % relative humidity with the coated panels in a 7.1 Wh D823 Test Methods for Producing Films of Uniform horizontal position while drying. listed in 7 (d'y Thickness of Paint, Varnish, and Related Products on Nab' 1--A device to equalize air change conditions has been between ti Test Panels3 developed by F. Scofield.6 Relative humidity should be controlled for 7.2 Set- D1005 Test Methods for Measurement of Dry-Film moisture-cured and two-package urethane coatings, since their cure is lightly tot Thickness of Organic Coatings Using Micrometers3 greatly affected by the existing moisture conditions. immediat D2091 Test Method for Print Resistance of Lacquers3 5.2 Tests should be carried out at practical viscosities at glass. Obs 2.2 U.S. Government Standards: which films can be applied to the proper film thickness with For the i Fed. Spec. No. CCC-C-440, Cheesecloth4 resultant good flow and leveling properties. In the absence of against th Fed. Spec. No. CCC-C-419b, Type HI, Army Duck4 any specific material specification, instructions for prepara transfer a 2.3 TAPPI Standards:5 tion of the film should be determined and agreed upon in cross S' T402 Standard Conditioning and Testing Atmospheres between the purchaser and the seller. tacky cor for Paper, Board, Pulp Handsheets, and Related Prod 5.3 Films to be tested should have practical thicknesses 7.3 Di ucts commensurate with performance characteristics expected 7.3.1 C 3. Significance and Use under actual usage for the type under test. All testing should individua be done within an area, any point ofwhich is not less than `/i 3.1 These test methods are used to determine the various in. (15 mm) from the film edge. stages and rates of drying, curing, and film formation of 5.4 Light Conditions--Illumination of the films during TABLE organic coatings for die purpose of comparing types of 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coalings and Materials and are the direct responsibility of the entire drying test period should be about 25 ft-candles (270 lx) from normal laboratory or sky sources, never from direct sunlight or other sources high in nonvisible radiant energy. Mate Drying c Varnish' Lacquer Resin s' Subcommittee D01.33 on Polymers and Resins. Current edition approved March 2J, 1983. Published July 1983. Originally published as D 1640 - 59 T. Last previous edition D 1640 - 69 (1974). 6. Preparation of Test Specimens 6.1 Carry out all tests as described in 6.1.1, 6.1.2 and Enamel.1 Oil pain Water p * Annua! Book ofASTMStandards, Vols 10.01 and 15.09. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 5 Available from Technical Association of the Pulp and Paper Industry, Technology Park, P.O. Box 105113, Atlanta, GA 30348. 6.1.3, unless otherwise noted. * Gardner and Sward, Paint Testing Manual, ASTM STP 500, ASTM, 1311 edition, 1972, p. 269. A This tat upon betwef a See 6.1 194 DUP050297377 T # D 1640 leant in isesand ngs not between ickness, coating oomor ducts of ght (see 3 2C tels in a has been rolled for ;ir cure is >sities at ess with ence of repara1 upon knesses xpected g should s than lh s during t-candles ver from ; radiant .1.2 and vSTM, 6.1.1 All test specimens shall be prepared and tested by o0e operator properly skilled in the methods to be used. Apply spec'1116118 >n duplicate at a time arranged so that examination intervals will fall within the normal working hours of the operator. 6.1.2 Apply the materials to be tested on clean glass panels or other specific substrate of suitable dimensions agreed upon between the purchaser and the seller. Groundg]ass plates are more suitable for certain types of coatings jjiat tend to crawl, such as low-viscosity drying oils. Suitable plates can be prepared by roughening the surface of polished glass by grinding a paste of silicon carbide (grit 1-F) and water between two glass plates. 6.1.3 The test films perferably shall be cast with a doctor blade having a clearance sufficient to give the recommended dry film thickness indicated in Table 1. When a suitable doctor blade is not available, or it has been agreed upon to apply &e film in some other manner, the various conven tional and automatic methods ofspray, dip, flow, and brush 1 application may be used, provided dry film thicknesses conform to the requirements given in Table 1. See Test [Methods D823 for a description of the spray and dip" methods of application. 6.1.4 Measure the dry film thickness of test films with the proper film thickness gage. This shall be a micrometer, dial comparator, or dial indicator as described in Test Methods D1005. When plates of small area are used, measurement of dry film thickness can be made by weighing plates before and after coating and calculating from plate area and coating solids. 7. Procedure 7.1 When test methods or end points other than those listed in 7.2 to 7.9 are used, there shall be a prior agreement between the purchaser and the seller. 7.2 Set-To-Touch Time--To determine set-to-touch time, lightly touch the test film with the tip of a clean finger and immediately place the fingertip against a piece of clean, clear glass. Observe if any of the coating is transferred to the glass. For the purpose of this test, the pressure of the fingertip against the coating shall not be greater than that required to transfer a spot of the coating from l/s to V\t> in. (3 to 5 mm) in cross section. The film is set-to-touch when it still shows a tacky condition, but none of it adheres to the finger. 7.3 Dust-Free Times: 7.3.1 Cotton Fiber Test Method--Separate a number of individual fibers from a mass of absorbent cotton with the TABLE 1 Recommended Film Thickness of Materials to be Tested4 Material Drying oils Varnishes . lacquers Resin solutions Enamels 09 paints _ Water paints Pry Film Thickness 1.25 0.25 mil (32 6 pm)s 1 0.1 mil (25 2 pm) (Sea 7.3.2) 0.5 0.1 mil (12.5 2 pm) (See 7.4.2) 0.5 0.1 mil (12.5 2 pm) 1.5 0.25 mil (36.5 6 pm) 1.8 0.2 mil (45 2.5 pm) (see 6.2) 1 0.1 mil (25 2 pm) This table is a general guide to be used when nothing more specific is agreed between the purchaser and the seller. "See 8.2 and 7.4.1. Add driers a minimum of 24 b before test; Ncd' --1 in. = 25.4 mm. FIG. 1 Typical Dust-Free Tester aid of tweezers. At regular drying intervals, drop several of the cotton fibers from a height of 1 in. (25 mm) onto a marked section of the film. The film is considered to have dried dust free when the cotton fibers can be removed by blowing lightly over the surface of the film. 7.3.2 Powder Test Method--Deposit finely divided cal cium carbonate (pigment grade) on the film at definite intervals during the drying period and, after the film has dried tack-free, remove by blowing with a gentle stream ofair and wiping with a soft rag or camel-hair brush. The coating is considered dust-free at the time interval when the pigment can be removed completely. 7.3.2.1 Deposit the calcium carbonate from a box through a 160-mesh screen in a pattern IV2 in. (40 mm) long and % in. (10 mm) wide. Fasten a vibrator to the side of the container to facilitate the passage ofthe pigment through the screen in a uniform pattern. Support the apparatus so that there is a clearance ofabout % in. (3 mm) between the screen and the test film. Figure 1 shows a typical dust-free tester7 and Fig. 2 shows the pattern obtained in testing a black enamel. The enamel shown is considered dust free at the 41/2-h rating. 7.4 Tack-Free Times: 7:4.1 Paper Test Method: 7.4.1.1 Test Paper--The test paper shall be K-4 Power Cable Paper8 that when conditioned in accordance with the TAPPI Standard Method T 402, conforms to the following requirements: 7 The dust-free tester was designed and built by Technical Subcommittee 37 of the New York Paint and Varnish Production Club and is described in "Investi gation ofMethods ofMeasuring Drying Time," Official Digest, Federation of Paint and Varnish Production Clubs, No. 286, November 1948, pp. 836-843. This paper also includes a study of the Zapon tack tester. 8 Paper meeting these lequirements may be obtained from Crocker Technical Papers, Inc., 431 Westminster St, Fitchburg, MA 01420, their Grade R 20-34. 195 DUP050297378 # D 1640 FIG. 2 Example Pattern from Dust-Free Drying Time Test Basis weight (24 by 36/500), lb Thickness, mils (pm) Air resistance (s/100 cm2/in.2) Coefficient of static friction * Friction angle, * Tensile strength, machine direction/cross direction Tear, machine direction/cross direction Elongation, machine direction/cross direction, % pH of water extract Ash content, max, % 90 5 6.65(17) 350 0.5 22 119/32 180/250 3.0/7.0 7.4 0.6 A AO tests except thus one shall be run in accordance with Test Method D 202. All values for properties are typical values and not specification limits. 7.4.1.2 Lay a 2 by 3-in. (50 by 75-mm) piece ofthe special test paper on the film and place upon it a steel cylinder 2 in. in diameter, and of such weight 6.28 lb, (2.85 kg), as to produce a pressure of 2 psi (13.8 kPa). At the end of 5 s, remove the cylinder and invert the test panel. The film is considered free from after-tack when the paper drops off of the test film within 10 s. 7.4.2 A variation of the test method described in 7.4.1 using the same test paper can be used to test the tack-free time of insulating varnishes. In this method the piece of paper shall be 1 lh in. (40 mm) in width and 6 in. (150 mm) in length. The varnish is considered tack-free when this strip of paper does not adhere to it when it is pressed on the surface of the varnish for 1 min by a cylindrical 1-lb (450-g) weight, l in. (25 mm) in diameter. In this test, apply .the paper in the vicinity of the center of the specimen at right angles to the length of the coated specimen. 7.4.3 Mechanical Test Method (Tack Tester9)--The tack tester to be used in this method comprises essentially a base or surface-contacting portion 1-in. (25-mm) square and a counter-balancing portion 1 by 2 in'. (25 by 50 mm) in area. Both portions are made up from a continuous metal strip 9 The standard tack tester is fully described in the U. S. Patent 2,406,989, Sept. 3, 1946. 0.016 to 0.018 in. (0:41 to 0.46 mm) in thickness. To prepare the apparatus for use (see 7.4.3.1), fit the base with several thicknesses of masking tape and paper strips to provide a means of attaching the aluminum foil and so adjust the angle of the 1 by 2-in. counter-balancing strip so that a weight of 5 g placed in the geometric center of the base portion is just sufficient to overcome the unbalanced force. 7.4.3.1 The tester is prepared for use by carrying out the following steps in sequence: (1) Wrap the metal base with three thicknesses of masking tape, sticky side out, (2) Cover the outer layer with a good grade of paper, except for two exposed strips, equally spaced, about ]A by 1 in. (6.4 by 25 mm) in area on the top of the tester, and (J) Cover the paper on the contact side of the base with one thickness of pressure-sensitive cellulose tape previously fixed to the metal base ofthe tester. The cellulose tape serves two purposes: First, to pull the layers of masking tape firmly against the front of the metal base, and -- Second, to provide a smooth surface for the foil. Attach the aluminum foil to the base of the tester by pressing gently but firmly a 1 by 2-in. (25 by 50-mm) piece of foil, 0.0005 in. (13 pm) in thickness against one of the `4 by 1-in. (6.4 by 25-mm) exposed strips of masking tape on the top surface of the base. Wrap the foil tightly and smoothly around the base, exposing the shiny side, and finally press the outer end gently against the remaining exposed strip of masking tape. When it finally becomes necessary to replace wrinkled or soiled aluminum foil, the ends are easily removed from the masking tape by exerting a slow, even, upward pull sufficient to overcome the tack of the tape without tearing the foil. 7.4.3.2 A film is considered to have dried tack-free when the tack tester tips over immediately on removing a 300-g weight allowed to act for 5 s on the counter-weighted metal square base fitted with masking tape and aluminum foil. 7.5 Dry-To-Touch Time: 7.5.1 Drying Oils--Continue testing after the set-to-touch time has been observed. The film is considered dry when it no longer adheres to the finger and does "not rub up appreciably when the finger is lightly rubbed across the surface. 7.5.2 Lacquers (and Sealers)--Touch the film lightly at varying intervals of time. The film is considered dry when no pronounced marks are left by the finger touching the film in the same area on each observation. Test sealers on wood or other porous substrates as agreed upon between the pur chaser and the seller. 7.6 Dry-Hard'Time: 1.6.1 With the end of the thumb resting on the test film and the forefinger supporting the test panel,, exert a max imum downward pressure (without twisting) of the thumb on the film. Lightly polish the contacted area with a soft cloth. The film is considered dry-hard when any mark left by the thumb is completely removed by the polishing operation. 7.7 Dry-Through (or Dry-To-Handle) Time: 7.7.1 Place the test panel in a horizontal position at a height such that when the thumb is placed on the film, the arm of the operator is-in- a vertical line from the wrist to the shoulder. Bear down on the film with the thumb, exerting the maximum pressure of the arm, at the same time turning 196 the thui The filr there is evident 7.8 L 7.8.1 coat ors meet oi adhesior does noi coat. 7.9 P Nef' . that the ti Method I i 7.9.1 plane pa of wood upon be 7.9.2 forming cheesecl 7.9.2. made of weighing of the w 7.9.3 than 2 ii ular to t lb/in.2 (1 7.9.4 7.9.4.1 or agreec method, or multi] DUP050297379 0 prepare h several provide a the angje eight of 5 311 is just g out the ? masking of paper, t V4 by 1 and base with ireviously ipe serves ?ainst the il. Attach ng gently 3.0005 in. 1. (6.4 by surface of i the base, nd gently . When it or soiled from the sufficient te foil. 'ree when g a 300-g ted metal n foil. -to-touch v when it rub up ross the ghtly at vhen no 3 film in wood or the pur- D 1640 h, thumb through an angle of 90 in the-plane of the film. !jre gim is considered diy-througb or dry-to-handle when Lte is no loosening, detachment, wrinkling, or other \|jence of distortion of the film. 6 7.8 Dry-To-Recoat: j'g, 1 A film is considered diy for recoating when a second coat or specified topcoat can be applied without the develop ment of any film irregularities such as lifting or loss of Sbesion ofthe first coat, and the dry time ofthe second coat does not exceed the maximum specified (if any) for the first rost. 7.9Print-Free Time: 2--This procedure is similar to Test Method D 2091, except itst the time to reach the print-free condition is determined, while Test jjjgjliod D 2091 is used to evaluate whether a film is print free at a spedBed time. 7.9.1 Test Panels--Apply the material under test to clean ulsiie panels, at least 3 by 6 in. (75 by 150 mm) in size, made of wood, metal, glass, plastic or other material as agreed upon between the purchaser and the seller. 7.9.2 Imprinting Fabric--Eight-ounce Army duck conforming to Type III of U.S. Fed. Spec. No. CCC-C-419b or cheesecloth conforming to Fed. Spec. No. CCC-C-440. 7.9,2, l A pad should be used with the cheesecloth only, made of nonwoven felt cloth at least 0.05 in. (1.3 mm) thick, yfighing 7 oz/yd2 (0.24 kg/m2) and larger than the plane end of the weight 7.9.3 Weights--Consisting of metal cylinders not less than 2 in. (50 mm) in diameter with plane ends perpendic ular to the axis and of a length to give a pressure of 'h or 1 lb/in.2 (3.5 or 6.9 kPa). 7.9.4 Procedure: 7.9.4.1 Apply the test material to several of the specified or agreed-upon panels by a film applicator, or other specified method, as described in Test Methods D 823 in either single or multiple coats, as agreed upon between the purchaser and the seller. In the absence of a specified dry film thickness, the values listed in Table 1 should be used. 7.9.4.2 Allow the coated panels to dry under the condi tions specified in Section 5, unless otherwise agreed. At appropriate intervals, starting shortly before the coating is expected to be print-free, carry out the print-free test as described in Test Method D 2091, comparing the appear ance with the photographic standards appearing therein, until the test shows the coating to be print-free. 8. Frequency of Testing 8.1 It is suggested that test intervals be set at periods of approximately 10 % of the total test time. If frequency varies considerably from the 10 % interval or such time interval is impractical, the intervals used shall be reported. 9. Report 9.1 Reports of tests shall include all applicable conditions that deviated from the standards as outlined or special conditions or tests used and the results of the test. 10. Precision 10.1 Because of the subjective nature of the drying time tests, the agreement to be expected between laboratories depends upon their understanding of the terms used, and is difficult to establish with certainty. Within any laboratory, the agreement depends upon the material being tested, some coatings being much sharper in their end point than others, but duplicate determinations should agree within 10 % ofthe time of drying.10 11. Keyword 11.1 drying time ,0 See Plane, 3. W., "A Latin Square Drying Time Study." Paint Industry Magazine (August 1961), far a study of precision of drying time measurements. The American Society tor Testing and Materials takas no position respecting the validity at any patent rights assarted in connection with any gam mentioned hi this standard. Users of this standard are expressly advised that determination of the validtty of any such patent rights, and the risk of Infringement of suoh rights, are entirely their own responsibility. This standard is sub/ect to revision at any time by the responsible technical ccmmhtee and must be reviewed every five years and not revised, eitherreapproved or withdrawn. Your comments amInvHed either torrevision ofthisstandard orfor addhlonai standards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you fee! that your comments have not received a fair heating you should make your views known to the ASTM Ccmmhtea on Standards, 1916 Race St., Philadelphia, PA 19103. test film t a maxte thumb th a soft rk left by peration. tion at a film, the ist to the exerting e turning DUP050297380 Designation: D 1641 - 59 (Reapproved 1987) Standard Test Method for Exterior Durability of Varnishes1 This standard is issued under the fixed designation D 1641; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovaL 1. Scope 4.2 Application of First Coat--For the first coat, thin a 1.1 This test method covers the testing of the exterior portion of the varnish in the proportion of I pt of mineral durability of varnishes applied to a wooden base. spirits thinner to 1 gal (500 ml in 4 L) of varnish. Coat both 1.2 This standard may involve hazardous materials, oper sides,, ends, and all edges of the test panel, using a small f ations, and equipment. This standard does hot purport to brush and taking the precaution to brush the coat out well. address all ofthe safety problems associated with its use: It is Allow the varnish coat to dry 24 h at room temperature the responsibility of the user of this standard to establish before applying the second coat. i appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 4.3 Application of Second Coat--Before applying the second coat, lightly sand the panel with 180-grit sandpaper, and reweigh the panel. Record the final weight of the first 2. Referenced Documents .. coat. Do not touch the sides ofthe panel after sanding. Using 2.1 ASTM Standard: D962 Specification for Aluminum Powder and Paste Pigments for Paints2 2.2' Military Specification: MIL-V-16399 Varnish, Moisture-Proof3' the varnish as received, apply a second coat, covering both sides and all edges of the panel. Apply the second coat as evenly as possible. Allow it to dry for 24 h before applying the third coat 4.4 Application of Third Coat--Before applying the third coat, lightly sand the panel with 180-grit sandpaper, taking 3. Apparatus 3.1 Maple Panels, of close-grained clear maple, 3 by 12 by Vi in. (76 by 305 by 13 mm), with all edges rounded to a lii-in. (6.4-mm) radius. 3.2 Varnish Brushes, 1-in. (25-mm) pure bristle. 3.3 Sandpaper, 180-grit. 3.4 Balance, capable of weighing to an accuracy of 0.1 g. 3.5 Tung Oil Phenolic Aluminum Sealer, 12'/z gal (47.3 L) "oil length" (12l/2 gal of oil/100 lb (45.4 kg) of resin. care not to touch the sides of the panel after sanding. Weigh the panel, and record the weight of the second coat. Using the varnish as received, apply the third coat covering both sides and all edges df the panel. Apply this coat with a full brush, laying the varnish on as evenly as possible. Allow it to dry for 24 h. Weigh the panel, and record the weight of the third, and final coat. 4.5 Application of. Aluminum Sealer--Using the alu minum sealer supplied' with the varnish samples, coat one side and all' the edges ofthe panel with a smooth, even coat. Ngh' 1--This sealer is composed of a vehicle made in accordance with Military Specification MIL-V-16399 Type B, 27 June, 1951, plus aluminum paste meeting the requirements of Specification D 962, Type II, Class B, using: 1 gal MIL-V-16399 Type B varnish,3 and 2 lb Great care should be taken to see that the ends and edges of the panel' are Completely covered. Allow the panel to dry a minimum of 24 h before, exposure. aluminum paste. 5. Exposure r,i 4. Preparation of Test Panels 5.1 Expose all- panels outdoors in the early Spring at 45* ' facing south. The weather conditions at the site of exposure 4.1 Weight ofPanel--Weigh the test panel to the nearest should duplicate, if possible, the. conditions under which 0.1 g, prior to varnishing. varnish will be exposed in regular use. -I' 6. Panel Examination 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and are: the direct responsibility of Subcom mittee D03.33 on Varnish and Resins* Including Shellac. Current edition approved Sept. 10, 1959. Published November 1959. Replaces 6.1 Inspect the panels at monthly intervals after the initiation of the exposure test. Sponge off the panels with a pad of cheesecloth under a gentle stream of cold water, and Sections 56-60 of D 154. 2 Annua! Book cfASTM Standards, Vo! 06.02. 3 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. immediately dry thoroughly with a soft cloth or low-pressure stream of air. Examine each panel for the following failure characteristics, grading each type of failure from " 1" to "10," "1" S evider 6.1. 6.1. 6.1. 6.1. 6.1. 6.1. 198 DUP050297381 oat, thin of mine, Coat be ^8 ^ sm* it out we :mperatu P^mg the sandpaper Dfthefi^ tag. Using ering both od coat as e applying g the third per, taking ing. Weigh oat. Using ering both with a full Allow it to ightofthe ; the alucoat one even coat id edges of el to dry a # D1641 unifying complete failure, and "10" signifying no 'f ~of.failurecharacteristics. ^ 11 General appearance, 6-,2 Craddng, "',3 Checking, T,4 Dulling, ', 5 Discoloration, and *,6 Recoatability. 7. Report4 7.1 Report the results of the examination of the test panels in accordance with Section 6. 4 The cooperative, experimental results on which this method is based were published in the Official Digest, Federation of Paint and Varnish Production Clubs, April 1952, pp. 219 to 220. The American Society for Testing and Materials takes no position respecting the validity ofany patentrights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ofInfringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee end must be reviewed every five years and itnotrevised, eitherreepproved or withdrawn. Tour comments are Invitadalther tor revision of this standard or tor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful conslderetlon at a meeting of the responsible technical committeei which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Race Sr., Philadelphia, PA 19103. cP- ng, at 45* ' exposure ler which after the ids with a water, and w-pressure ing failure rto"io," 199 DUP0502 97382 (jjjjM Designation: D1642 - 70 (Reapproved 1087} Standard Test Methods For Elasticity or Toughness of Varnishes1 This standard is issued under the fixed designation D 1642; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. These methods have been approvedfor use by agencies ofthe Department ofDefense to replace Methods 4151, 4152 ofFederal Test Method Standard No. 141 andfor listing in the DoD Index cfSpecifications arid Standards. with hi-fl amber git 4. Test P 4.1 Tes plate weig i f25 or lesf l shall be wi ! 3 by 5 in. with benz : buffed) an 1. Scope 1.1 These methods cover the determination ofelasticity or toughness of any varnish which is miscible with the diluents specified, under the conditions ofthe test. 1.2 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Summary of Methods 2.1 Elasticity or toughness of the varnish may be deter mined by proportionately reducing its elasticity or toughness by the addition of a standard solution of a resin. The .long-accepted use of run-kauri gum may now be less convenient due to a limited supply ofthis resin. Accordingly, an equally acceptable resin is prescribed in Method A (Sections 3 to 6). Method A is based on the preparation of a rosin-pentaerythritol ester, the properties of which in terms of acid value and melting point can be controlled, and on a solvent that is free of any inherent polymerization tendency. Where desired, run-kauri gum may be used as prescribed in Method B (Sections 7 to 9). 2.2 For varnishes that are less elastic or tougher than zero standard resin reduction, Method C (Sections 10 to 13), based on proportionately increasing the elasticity or tough ness of the varnish by means of the addition of linseed oil, is provided. METHOD A--STANDARD ROSIN PENTAERYTHRITOL ESTER RESIN REDUCTION 3. Preparation of the Rosin-Pentaerythritol Ester Solution 3.1 Apparatus: 3.1.1 Flask, 3-litre, 3-neck flask. 3.1.2 Gas Burner having a capacity of 12 000 Btu/h (3.5 kW). 3.1.3 Agitator--Motor-driven agitator with blade periph eral speed of 600 ft (182.9 m)/min. The agitator shall be of the three-blade type with a blade width of V* in. (19 mm) and a blade diameter of 1% in. (44.5 mm). 3.1.4 Thermometer--An ASTM Partial Immersion The, mometer having a range from 20 to 760 F, 16 in. (406 in length, and conforming to the requirements for TW mometer 3F in ASTM Specification El, for ASTM Thermometers.2 3.1.5 Carbon Dioxide Supply. 3.2 Materials: 3.2.1 W. W. Gum Rosin: Melting point Acid number 173 to 177F(78to31Q 165 to 167 3.2.2 Pentaerythritol: Hydroxyl content Ash content Melting point 49.5% less than 0.2% at least 250 C 3.2.3 Hi-Flash Naphtha: Type Color Distillation range Dry point Add wash color Spedfic gravity 15.56/15.56 C Flash point (Tag open cup) aromatic water-white first drop not below ISO C not above 193 C not darker than No. 10 color standard3 0.855 to 0.890 105 F (40.66 Q 3.3 Procedure--Heat 3 lb (1361 g) of rosin in the I fitted with the thermometer, a carbon dioxide inlet ratmifini I below the surface of the reacting liquid, and a loose call stuffing box fitting the center neck of the flask through which is extended the agitator shaft. When the rosin reaches i j temperature of 450 F (232 C), start the motor stirrer, i the C02 flow so that about two bubbles break to the surface 1 per second, and add 0.33 lb (150 g) of pentaerythritol slowff through the center neck while keeping the agitator runnhig [ The size of the hole in the cork accommodating the agitata shaft should be large enough to allow the escape ofC02 and ] water vapor from the flask and prevent any pressure brnklj up. After all of the pentaerythritol has been added, heat to l 600 F (315 C) and hold for an acid number of S. Hfj softening point should be about 263 F (128 C) as determittil by the Test Method for Softening Point by Ring and BH Apparatus (ASTM Designation: E 28).4 The time requind*! about 6Vi h at this temperature. When the resin reachestj*| correct acid number and melting point, turn off the Allow the carbon dioxide to flow until the flask has cooled#! 400 F (204 C), then pour the liquid resin into a tared recall and carefully reduce to 33 VS % nonvolatile matter cofiWjf ' 5. Procedi 5.1 Red nonvolatile described i Content of and add t< equivalent the nonvol the solutior 5.2 Appl reduced vai 4. Let stand 70 to 90 F horizontal j for 5 h at 20 the oven an 5.3 Bend. panel over supports. W it in positioi the top and double in I Examine the diameters, u; 6500 K and (hose not eqt panel at a no sky will appr over the ben each side of i 6. Report 6.1 Report test as passin ^Jecified. 6-2 If a lin eentage is desi reduction, ba; garnish, shall For example, standard resin ME' Peepars 1 These methods are under the jurisdiction of ASTM Committee 0-1 on Paint and Related Coatings and Materials and are the direct responsibility of Subcom mittee DO 1.33 on Varnish and Resins, Including Shellac. Current edition effective Dec. 24, 1970. Originally issued 1959. Replaces D 1642 - 59. Replaces Sections 20-32 of D 54. 2 Annual Book qfASTM Standards, Vols 05.03 and 14.01. 'ASTM Method D848, Test Method for Acid Wash Colot oft Aromatic Hydrocarbons, see Annual Book ifASTMStandards, Voi 16.03. 4 Annual Book ofASTM Standards, Vol 06.03. > Wei i able size a Annual Book , 200 DUP050297383 n Ther)6 mm) r TherASTM Q oc be flask tending >se cork b which aches a % adjust surface slowly inning, igitator 02and : buildheat to 8. The jrmined ind Ball luired is ches the he heat, ooledto receiver content ' Industrial 5.03. # D 1642 tfith hi-flash naphtha. Store the solution in tightly-closed amber glass bottles. 4, Test Panels 4.1 Test panels shall be No. 31 gage (0.227 mm) bright tin plate weighing not more than 0.51 nor less than 0.39 lb/ft2 (25 or less than 19 g/dm2). It is important that the tin plate shall be within the limits prescribed. The panel shall be about 3 by 5 in. (76 by 120 mm) and shall be thoroughly cleaned vdth benzene immediately before using (cleaned but not buffed) and wiped dry with a clean cloth. j. Procedure 5.1 Reduction of the Varnish--Carefully determine the nonvolatile matter content of the varnish under test, as described in ASTM Methods D 1644, Test for Nonvolatile Content of Vamishes.s Then take at least 10 g of the varnish and add to it an amount of the standard resin solution equivalent to the specified percentage reduction by weight of the nonvolatile matter in the varnish. Mix the varnish and the solution thoroughly. 5.2 Application of Reduced Varnish--Flow a coat of the teduced varnish on one ofthe tin panels described in Section 4, Let stand in a nearly vertical position at room temperature 70 to 90 F (21 to 32 C) for 1 h. Place the panel in a horizontal position in a properly ventilated oven and bake for 5 h at 203 to 212 F (95 to 100 C). Remove the panel from the oven and allow to cool at 77 F (25 C) for 30 min. 5.3 Bending of Test Panel--Quickly bend the coated panel over a %-in. (3-mm) rod held firmly by suitable supports. With the coated side ofthe panel uppermost, place it in position on the rod so that the rod is equidistant from the top and bottom edges of the panel. Bend the panel double in 1 s at a temperature of 77 0.2 F (25 0.1 C). Examine the film at the bend under a magnification of 5 diameters, using diffused light having a color temperature of 6500 K and intensity of about 165 ft-candles (1770 be). (For those not equipped with a standard illuminant, viewing the panel at a north window illuminated by a farily light overcast sky will approximate these conditions.) No cracks shall occur over the bent area between the points lA in. (6.4 mm) from each side of the panel. 6. Report 6.1 Report varnishes that do not show cracks under this test as passing the percentage of standard resin reduction specified. 6.2 If a limiting percentage rather than a specified per centage is desired, successive changes of 10 % standard resin reduction, based on the nonvolatile matter content of the varnish, shall be made until a limiting percentage is found. For example, varnishes may be reported as passing 40 % standard resin reduction and breaking at 50 %. METHOD B--RUN-KAURI REDUCTION 7. Preparation of Standard Run-Kauri Solution 7.1 Weigh into a side-tube type distillation flask of suit able size an amount of clear, hard, bright pieces of "No. 1 Grade" kauri gum, equivalent to approximately one third of the volumetric capacity of the flask. Attach the flask to a water-cooled condenser. Carefully melt and distill the gum, collecting the distillate in a tared receiver. Stop the distilla tion when 25 % by weight of the gum has been collected in the tared receiver. A thermometer so placed in the distilling flask that its bulb is level with the discharging end of the flask should read about 600 F (316 C) at this point. Pour the residue in the distillation flask into a clean pan, and when cool break it up into small pieces. 7.2 Place in a tared beaker a given weight of the small pieces ofthe run-kauri gum, which shall be free from all dust or powder, together with twice its weight of freshly distilled gum spirits of turpentine conforming to ASTM Specification D 13, for Spirits of Turpentine,4 using only that portion distilling between 307 and 338 F (153 and 170 C). Dissolve the gum in the turpentine by heating the contents of the beaker slowly to a temperature of 302 F (150 C). The contents Of the beaker should be stirred occasionally to prevent the sootened gum from adhering to the bottom ofthe beaker, thus avoiding possible over-heating of the gum and facilitating its solution. Allow the solution to cool to between 167 and 212 F (75 and 100 Q and filter through a fluted filter paper into a previously weighed, clean, brown glass bottle equipped with a screw cap. 7.3 Examination of Run-Kauri Solution for Solvent Compatibility--To 5 ml of the run-kauri solution in a clean, clear glass tube add 5 ml of mineral spirits conforming to ASTM Specification D 235, for Petroleum Spirits (Mineral Spirits),4 and in addition having an aniline point of between 55 and 60 C determined in accordance with ASTM Method D 611, Test for Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents.6 Mix thor oughly and allow to stand for 1 h at room temperature, between 70 and 90 F (21 and 32 Q. At the end of 1 h the mixture shall be completely miscible and show no clouding, precipitation, or separation. If clouding, precipitation, or separation occurs, the run-kauri solution shall be considered unsatisfactory for use. 7.4 Adjustment ofRun-Kauri Solution to Proper Nonvola tile Matter Content--Transfer 10 to 15 ml of the filtered run-kauri solution to a stoppered flask or weighing pipet and determine the percentage of nonvolatile matter as described in Methods D 1644, with the following modifications: Add approximately 2 g of raw castor oil, accurately weighed, to each 80-mm dish or lid before adding the run-kauri solution and heat for 3 h at 115 2 C. At least three determinations shall be made, using samples of run-kauri solution weighing 1.2 0.1 g, and at least two blanks shall be run on the castor oil alone under the same conditions to determine its loss in weight Calculate the nonvolatile matter content of the run-kauri solution, making allowance for the loss in weight of the raw castor oil. From the average nonvolatile matter content thus determined and the weight of the run-kauri solution, calculate the amount of freshly distilled gum spirits of turpentine required to adjust the nonvolatile matter content of the run-kauri solution to 33.3 weight %. After the 3 Annual Book ofASTM Standards, Vol 06.01. 6 Annual Book ofASTM Standards, Vol 05.01 and 06.03. 201 DUP0502 97384 D 1642 addition ofthe required amount ofthe turpentine, repeat the nonvolatile matter determination and record the nonvolatile matter content, which shall be 33.3 0.1%. 8. Procedure 8.1 Using test panels prepared as in Section 4, and run-kauri solution as in Section 7, follow the procedure described in Section 5. 9. Report 9.1 Report as directed in Section 6, expressing the results in terms of run-kauri reduction instead of standard resin reduction. METHOD C--ADDITION OF UNSEED OIL 10. Scope 10.1 This method is applicable to varnishes that are less elastic or tough than zero standard resin reduction. It is identical with that described in Method A, except that the 33% % solution of standard resin in hi-flash naphtha i$ replaced by a 66% % solution of heat-bodied linseed oil for proportionately increasing the elasticity of the varnish under test 11. Preparation of Standard Bodied Oil Solution 11.1 Heat a high grade of alkali-refined linseed oil having an acid number less than 1.0 in an open kettle at a temperature of 300 5 C until the viscosity of the oil after cooling is between 6 and 10 St (0.0006 and 0.0010 m2/s) at 77 F (25 C). 11.2 Standardize a quantity of the heat-bodied linseed oil by reducing it with one half its weight of pure redistilled turpentine conforming to Specification D 13,4 using only that portion of the turpentine distilling between 307 and 338 F (153 and 170 C). 12. Procedure 12.1 Prepare the test panels and perform the addition of the standard bodied oil solution to the varnish and the flowing on, baking, and bending of the test panel exactly as described in Section 5. 13. Report 13.1 Report the minimum percentage of the oil solution that must be added to the varnish, based on its nonvolatile matter content, so that the final mixture when flowed on a test panel and-baked does not crack on the subsequent bending over a 3-mm rod. 14. Precision 14.1 The precision of this method is limited by the character of the testing ingredients and procedures and the interpretation and visual observation of the results. These, results are not specifically numerically oriented and, there fore,, .comparison with standards of control materials known to have acceptable properties, determine the precision. The American Society for Testing and Materials takes no position respecting the validity at any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ot any such patent rights, and the risk of Infringement Of such rights, are entirely their own responsibility. This standard Is subject to revision at any time try the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invitedeither for revision of this-standard orfor additional standards end should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your, views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ' a. ati a. a 202- K. 'is-: i: r r.- DUP050297385 `seed oij distilled n8 omy *07 and lition of and the cactly as solution tvolatile 'ed on a >sequent by the and the s. These i, theres known jn. Designation: D 1643 - 60 (Reapproved 1988) Standard Test Methods for Gas Checking and Draft Test of Varnish Films1 This standard is issued under the fixed designation D 1643; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapprova). A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. j. Scope 1. l These test methods cover the determination of the gas pecking and draft test of varnish films. 1.2 This standard may involve hazardous materials, oper- gions, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is die responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2, Referenced Document 2.1 ASTM Standard: D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature2 GAS CHECKING 3, Scope 3.1 This test method3 covers two alternative procedures for detecting nonuniform appearance that may develop while a film of varnish dries in an atmosphere that has been fouled by products of combustion. The nonumform appear ance is generally related to wrinkling, which is sometimes microscopic and which is variously described as checking, crow's-footing, crystallization, or dulling. Appearance non uniformities that develop on dried films and are described by such terms as orange-peel, haze, silking, flooding, etc., arenot within the scope of this test method. 4. Summary of Test Method 4.1 The varnish film under test is exposed to foul. gas for various periods before the film has been' converted from liquid to substantially solid, since the foul gas is effective, within the scope of these test methods, only before the varnish film has become set-to-touch or dust-free. 1 These test methods are under the jurisdiction of ASTM Committee EM on Paint and Related Coatings and Materials and the direct Responsibility of Subcommittee D 01.33 on Varnish and Resins, Including Shellac. Current edition approved Sept. 19, I960. Published November 1960. Originally published as D 1643-59 T. Last previous editions D 1643-59 T. Replaces Scions 2 to 14 of Method D 154. 2 Annual Book ofASTM Standards, Vol 06.01. 'See JPaint Testing Manual. ASTM STP 500. ASTM, 1972. PROCEDURE A--BELL JAR TEST 5. Apparatus 5.1 The form and arrangement of the apparatus shall be designed to provide an even distribution of the products of combustion over die test panels. 5.1.1 Glass Bell Jar, approximately 8 in. (203 mm) in diameter and 12 in. (300 mm) in height, inside dimensions, having a ground-glass rim. 5.1.2 Ground-Glass Base Plate, of suitable size. 5.1.3 Metal Frame, fitted inside the bell jar and provided with a suitable support for holding a tin-plate disk 6 in. (152 mm) in diameter in a horizontal position 2 in. (51 mm) above the wick of the lamp. 5.1.4 Additional Horizontal Supports, for holding the various varnished panels under test. 5.1.5 Small Kerosine Glow Lamp, without a chimney, or a small alcohol lamp filled with kerosine, using a round wick not over `A in. (6.4.mm) in diameter and adjusted to give a flame of Vs in. (20 mm) in height. 5.1.6 Tin-Plate Panels, 3 by 5 in. (76 by 127 mm) or smaller, cut from commercial No. 31 gage (0.227 mm) bright tin plate, weighing 0.39 to 0.51 lb/ft2 (1.9 to 2.5 kg/m2) and carefully cleaned with toluene and dried before use. 6. Procedure. 6i 1 Determine the normal set-to-touch or dust-free drying time of the varnish under test in accordance with Test Methods D 1640. Divide this time by five to arrive at the different drying periods at which the material is to be tested. Thus, if a .material sets to touch in 1 h, test the specimens for resistance to gas at drying periods of 12, 24, 36, and 48 min, .respectively,. 6.2 Flow the varnish to be tested on the tin-plate panels at the determined intervals of time. Allow the panels to drain in a nearly vertical position at room temperature 65 to 75F (18 to 24C). 6.3 After the required interval of drying time has passed, place the panels in a horizontal position on the upper supports of the frame. Light the lamp and place it on or near the center ofthe ground-glass base plate. After the bell jar has been placed tightly over the frame and lamp, the flame should extinguish in about 4 min. 6.4 Remove the panels and examine for gas effects after they have remained in the jar for 30 min. 7. Report 7.1 Describe the presence or absence of gas effects on the test panel for each drying interval. 203 DUP0502 97386 D 1644 Diameter of Dish Weight of Nonvolatile Residue 45 mm 100 mm For a 2.5-mil varnish film For a 5-mil varnish Sim 0.12 g 0.25 g O.SOg 1.20 g 8.2 Place the dish on the hot plate at 150 3.5C for 10 min. Cool to room temperature in a desiccator, then re weigh. 9. Calculation 9.1 Calculate the nonvolatile matter as described in Sec tion 5. 10. Report 10.1 Report the nonvolatile matter of the sample to th nearest 0.1%. ' e INDEX TERMS 11. Index Terms 11.1 These test methods are indexed under the folio* terms: nonvolatile matter content; varnishes. The American Society for Testing and Materials takes no position respecting the validity of any patentrights asserted In connection with any Item mentioned In this standard: Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Yourcomments are invitedeither forrevision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting at the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you.shouid make your views known to the ASTM Committee on Standards, 1918 Race St, Philadelphia, PA 19103. j. Scope 1.1 T1 resistanc dilute all 1.2 Tr Otions, c address t the respt appropru applicabi 2. Refer* 2.1 At D609 Pain D 119; D392* ditio Rela 3. Summ 3.1 Te onto tinp immersec other agr< 3.2 Te glass test then sust ranging fi 30 min, t 4. Signifi M<S.t f aI 4.1 Dr tion for solutions protective comparisc determine alkali. ! 5. Reager M 5.1 Put used in a) 206 DUP050297389 Designation: D 1647 - 89 Standard Test Methods for Resistance of Dried Films of Varnishes to Water and Alkali1 This standard is issued under die fixed designation D 1647; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reappraval. 1. Scope j i These test methods cover the determination of the i^ance of dried varnish films to immersion in water and jute alkali at room temperature. 1,2 This standard may involve hazardous materials, oper- gions, and equipment. This standard does not purport to ttfress all ofthe safety problems associated with its use. It is T, responsibility of the user of this standard to establish impropriate, safety and health practices and determine the applicability ofregulatory limitations prior to use. 2, Referenced Documents 2.1 ASTM Standards: 0609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D1193 Specification for Reagent Water3 D3924 Specification for Standard Environment for Con ditioning and Testing Paint, Varnish, Lacquer, and Related Materials2 }, Summary of Test Methods 3.1 Test Method A--The material under test is flowed onto tinplate panels and dried for 48 h. The panels are then immersed to half their length in reagent water for 18 h, pr other agreed upon time, removed, and examined visually.'s 3.2 Test Method B--The material under test is applied* to glass test tubes by dipping and dried for 72 h. The tubes are then suspended in dilute sodium hydroxide for periods ranging from 1 to 24 h, removed, rinsed, and after drying for 30 min, examined visually. 4. Significance and Use 4.1 Dried Varnish Films are a source of primary protec tion for surfaces. Exposure to water and dilute alkali solutions are two factors which tend to break down this " protective coating. This test method can be used as a ' comparison basis between manufacturer and consumer to determine the ability of the varnish to resist water and dilute alkali. that all reagents conform to the specifications of the Com mittee on Analytical Reagents of the American Chemical Society, where such specifications are available.4 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type IV of Specification D 1193. TEST METHOD A--WATER RESISTANCE OF DRIED FILMS 6. Apparatus and Materials ' 6.1 Beaker, glass, 600 mL or larger. 6.2 Tinplate Panels, 3 by 5 in. (75 by 125 mm) cut from commercial No. 3.1 gage (0.225-mm) bright tin plate, weighing 0.4 to 0.5 lb/ft2 (1.90 to 2.50 kg/m2) and carefully cleaned and dried before use in accordance with Methods B or C of Methods D 609. 7. Procedure 7.1 Flow the varnish onto the tin panels, allow to drain in a nearly vertical position, and dry for 48 h in the standard atmosphere described in Specification D 3924. 7.2 Place the panels in a beaker containing about 2.5 in. (65 mm) ofwater at room temperature, immersing the ends that were uppermost during drying, and allow to remain in the water for 18 h, or other suitable period as agreed upon between the purchaser and the seller. 7.3 Remove the panels from the water, wipe carefully, and allow to dry at room temperature. Note the time required for whitening, if any, to disappear. Blooming, which sometimes occurs on irtfihersion, is considered a type of whitening. 8. Report 8.1 Report the results of the water test as follows: 8.1.1 Not visibly affected, 8.1.2 Whitening disappears within 20 min, 8.1.3 Whitening does not disappear within 20 min, but disappears within 2 h, 8.1.4 Whitening does not disappear within 2 h, but disappears within 24. h, or 8.1.5 Whitening does not disappear within 24 h. 5- Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended 1 These test methods are under the jurisdiction of ASTM Committee D-1 on Kit and Related Coatings and Materials and are the direct responsibility of ^committee DO 1.33 on Polymen and Resins. Current edition approved April 28, 1989. Published June 1989. Originally MiKshed as D 1647 - 59. Last previous edition D1647 - 83. 2 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.03 and 11.01. TEST METHOD B--DILUTE ALKALI RESISTANCE OF DRIED FILMS 9. Reagent 9.1 Sodium Hydroxide Solution (30 g/L)--Dissolve 30 g 4 "Reagent Chemicals, American Chemical Society Specifications,'' Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 207 DUP050297390 D 1647 of sodium hydroxide (NaOH) in water and dilute to 1 L. 10. Procedure 10.1 Thoroughly clean and dry twenty 1 by 6-in. (25 by 150-mm) test tubes in toluene. Dip the tubes into the varnish under test, remove immediately, invert the tubes, and allow the varnish to dry for 72 1 h in the standard atmosphere described in Specification D 3924. A suggested test schedule to fit into normal working hours is shown in Table 1. 10.2 Into each of ten 1000-mL, tail-form lipless, chemi cally resistant plastic or glass beakers, place 300 mL of the NaOH solution. Suspend a set oftwo varnish-coated tubes in each beaker so that the tubes do not touch the bottom or sides of the beaker and are immersed for a distance of approximately 2 in. (50 mm). As a suspending device (see Fig. 1), use a wooden cover plate and two dowels, and two one-hole cork stoppers, the dowels and the corks fitting into the tubes and the cover plate fitting the beaker as tightly as possible. Maintain the NaOH solution at a temperature of 23 2C. 10.3 Remove a set of two varnish-coated tubes after immersion for each of the following time periods: 1, 2, 3,4, 5,6,7, 8,16, and 24 h. Rinse the tubes under a gentle stream of water, allow to air-dry for 30 min, and examine for film Day Monday Thursday Friday TABLE 1 Suggested Test Schedule Hour Operation 8:30 a.m. 4:00 p.m. 8:30 a.m. 9:30 am. and each hour thereafter to 4:30 p.m. 10:00 a.m. and each hour thereafter to 8:00 p.m. 4:00 p.m. 8:00 am. 8:30 am. 4:00 p.m. 4:30 pm. coal 16 tubes coat 4 tubes dry tubes for 72 h start alkali immersion on first 16 tubes remove one set of tubes from alkali, rinse, and air-dry for 30 min examine varnish film on set'of tubes removed Va h earlier start alkali immersion on last 4- tubes remove one set of tubes from alkali, rinse, and air dry for 30 min examine varnish film on set of tubes removed and rinsed % h earlier remove last set of tubes, rinse, and air-dry for 30 min examine varnish film on last sat of tubes Nij' --1 in. - 25.4 mm. FIG. 1 Apparatus for Alkali Resistance Test whitening, blistering, or removal. The end point of the test is the number of hours immersion at which the first signs of film whitening, blistering, or removal are noted on the vertical sides ofthe tubes or on the spherical bottom portion of the tube. The results may be compared with those from materials known to give acceptable performance. For referee work, the test on materials known to be acceptable should be made simultaneously. V S' 11. Report 11.1 Report the results of the alkali test as follows: 11.1.1 Type of varnish, and 1.1.1 .2 End point of the test, h. 12. Precision 12.1 Precision has not been determined due to the multi plicity of ambient test conditions. JJje American Society tor Testing amt-Materlals takes noposition respecting the validityofany patent rights asserted In connection with any item mentioned la this standard. Users ot this standard are express// advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee end must be reviewed every live years and Ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 181S Race St., Philadelphia, PA 19103. 1. I 1 at v lacc filer 1 1 1 1 obU app 1 desi fact 1. prol bilit safe regu 2. I 2. D E E :! 5 208 DUP050297391 Designation: D 1653 - 91a i test is igns of on the portion e. from referee ouldbe muiti- Standard Test Methods for Water Vapor Transmission of Organic Coating Films1 This standard is issued under the fixed designation D 1653; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of Jast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. These test methods have been approved for use by agencies of the Department of Defense to replace Method 6171 of Federal Test Method Standard No. 141A. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue that has been adopted by the Department ofDefense. 1. Scope i. 1 These test methods cover the determination ofthe rate at which water vapor passes through films of paint, varnish, lacquer, and other organic coatings. The films may be free tarns or they may be applied to porous substrates. 1.2 Two test methods are covered as follows: 1.2.1 Test Method A--Dry Cup Method, and 1.2.2 Test Method B--Wet Cup Method. 1.2.3 Agreement should not be expected between results obtained by different methods. The method that most closely approaches the conditions of use should be selected. 1.3 The values stated in inch-pound units are to be designated as the standard. Metric-inch pound conversion factors are stated in 13.2.1.2 and 13.2.2.2. 1.4 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsi bility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1ASTM Standards: D823 Test Method for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1193 Specification for Reagent Water3 D4708 Practice for Preparation of Free Films of Organic Coatings2 E 104 Practice for Maintaining Constant Relative Hu midity by Means of Aqueous Solutions4 inch-pound unit is grains per square foot per hour. Accepted SI unit is grams per square metre per 24 h. 3.1.2 water vapor permeance, WVP--the steady water vapor flow in unit time through unit area of a body (WVT) induced by unit vapor pressure difference (Ap) between the two surfaces .of a coating. Therefore, WVP = WVT/Ap. Accepted inch-pound unit is grains per square foot per hour per inch of mercury (called a perm). Accepted SI unit is grams per square metre per 24 h per millimetre of mercury (called a metric perm). 4. Summary of Test Methods 4.1 In Test Method A (Dry Cup Method), the test specimen is sealed to the open mouth of a cup or dish containing desiccant, and the assembly placed in a test chamber with a controlled atmosphere. Two sets of exposure conditions are acceptable for this test method. 4.1.1 Condition A, consisting of 50 % relative humidity at 73F (23C), and 4.1.2 Condition B, consisting of 90 % relative humidity at 100'F (38C). 4.2 In Test Method B (Wet Cup Method), the test specimen is sealed to the open mouth of a cup or dish containing water, and the assembly placed in a test chamber with a controlled atmosphere. Two sets of exposure condi tions are acceptable for this test method: 4.2.1 Condition A, consisting of 50 % relative humidity at 73F (23C), and 4.2.2 Condition C, consisting of very low (near zero) relative humidity at 73F (23C). 4.3 In both methods, periodic weighings ofthe cup or dish are made to determine the rate of water vapor movement through the specimen. 3. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 water vapor transmission rate, WVT--the steady water vapor flow in unit time through unit area of a body, between two specific parallel surfaces, under specific condi tions of temperature and humidity at each surface. Accepted 1 These lest methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.23 on Physical Properties of Applied Paint Films. Current edition approved Sept. 15,1991. Published November 1991. Originally Published as D 1653 - 59 T. Last previous edition D 1653 - 91. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. * Annual Book ofASTM Standards, Vol 11.03. 5. Significance and Use 5.1 One of the factors affecting the performance provided by organic coating is the degree of resistance to the passage ofwater vapor. Hence, the water vapor transmission characteristics of coatings are important in assessing their performance in practical use. 5.2 The purpose of these test methods is to obtain values of water vapor transfer through coatings that range in permeability from high to low. These values are for use in design, manufacture, and marketing. 5.3 The water vapor transmission is not a linear function of film thickness, temperature or relative humidity. 5.4 Values of water vapor transmission rate (WVT) and water vapor permeance (WVP) can be used in the relative 209 DUP0502 97392 D 1653 rating of coatings only if the coatings are tested under the 7.4 Release Paper, prepare free films, whenever possible 10. Pri same closely controlled conditions of temperature and rela tive humidity, and if their thicknesses are equal. 6. Apparatus 6.1 Perm Cup5 or Dish, consisting of a container made of a noncorroding material, impermeable to water or water vapor. If the cup or dish is made of aluminum, it must be anodized or given a protective clear coating to prevent to eliminate the potential interference of substrates, on release paper6 or glass substrates following procedures out lined in Practice D 4708. 7.5 Film Support) for preparing films that are too brittle or otherwise unsatisfactory for handling as free films, support materials such as paper charts,7 *filter paper, and glass cloth have been found satisfactory in some instances. Such support can have an effect on the test results. 10.1 test ma 10.1. of the t. 10.1.1 specime it firmh 10.1.1 corrosion. 6.1.1 One type of cup that is suitable has a flanged edge and is equipped with a separate corresponding flange, so that the test specimen can be held between them. The contacting faces ofthe flanges shall be ground to sufch flatness thatwhen the film is in position, moisture transfer can occur only through the exposed film area. For hard films, or films 8. Test Specimens 8.1 It is very important that the test specimens be smooth, and completely continuous films of uniform thickness throughout the test area. Apply air dry coatings to substrates using one of the methods described in Test Methods D 823 or Practice D 4708; test spec 10.1.3 size of t wax. 10.1J mouth c the cup having a very rough surface, a soft rubber gasket tnay be Nmn' 2--Special test conditions may require that the coating in coating inserted between the film and' the flange. The flanges shall applied by brushing, roller coating or other special methods. The away frc iSi then be held together with suitable clamps. 6.1.2 Another suitable cup is any open circular dish to which the test film can be sealed with wax or sealant. 6.2 Test Chamber, with a controlled temperature and relative humidity as specified in Section 4. Atf shall be circulated throughout the chamber to maintain uniform conditions at all test locations. For low or high humidity conditions, a standard desiccator or other suitable cabinet may be used. For maintaining constant relative humidity by means of aqueous solutions, refer to procedures outlined in Practice E 104. 6.3 Analytical Balance, having an adequate capacity far the weight of the test cups and a sensitivity of 1 mg. thickness ofthecoating applied shall be within normal range for the type of material under test, end shall not vary by more than 5 % of the total thickness in any test, series.. Nop' 3--When applying bake finishes, bake for specified time temperature in accordance with manufacturers' instructions. Permeant* may vary with the baking schedule or the time of air drying. 8.2 Air dry the coated material ii a horizontal position for 7 days in a room preferably maintained at 73.5 3.5F (23 2C) and 50 5 % relative humidity. If the material' to h used is a free film, remove it from the substrate and allow tfif previously unexposed surface to dry for an additional 7 days; The drying schedule may be modified as recommended by manufacturer. Nqr' 4--Examine test film for the presence of pinholes or olte Nmn' ; produce i always rui 10.4 \ test cabi relative I 10.5 F weight g; over 10 f once a dt 10.6 Ii 3 weeks. Record tl 7. Reagents and Materials defects before commencing the test. It may be advisable to apply the test approxiir 7.1 Purity of Water--Unless otherwise indicated, refer material in two coats, applying the second coat perpendicular to the fa Thus, if v coat and allowing for an adequate dry period between coats to achieve 15 minut ence to water shall be understood to mean reagent water the desired film thickness. 10.7 SI conforming to Type IV of Specification Dri'193. 8.3 Measure the thickness of the test specimen in seven! surface sr 7.2 Desiccant, consisting of either anhydrous calcium places with a micrometer using procedures in Test Methods the desia chloride (CaCL2) or anhydrous magnesium perchlorate D 1005 to ensure a uniform thickness. tinue the (Mg(CL04)2). The calcium chloride should be dried at 400F (200C) before use. Ifcalcium chloride will react with the test : 8.4 When coatings are applied to support materials, Ik 10.8 ft coated side of the test specimen should be placed,away from after weij specimen, an adsorbing desiccant such as a silica gel may be the desiccant or towards the water in the cup, depending used but the moisture gain by this desiccant during the test upon use. Coatings should not be applied to- both sides ofa must be limited to 4 %. Use caution in handling'magnesium perchlorate because of possible chemical reaction that may support. Glass cloth is preferred for coatings that are' cured by baking. ' 11. Test be produced if it comes in contact with some organic 11.1 U materials. - TEST METHOD A--DRY CfoP METHOD purchaser 7.3 iSealant, such as wax for attaching the test specimen to the top of the perm cup or dish. It must be highly resistant to 9. Test Conditions more of tl ; 11.1.1 t the passage of water vapor. It must not lose weight to, or gain 9.1 Unless other conditions are agreed upon between U* at 73 1 weight from, the atmosphere in an amount, over the purchaser and the seller, the tests shall be .performed unik ' 11.1.2 ( required period of time, that would affect the test results by one or more of the following conditions: <occ j tained at more than 2 %. It must not affect the. vapor pressure in a 9.1.1 Condition A---Test chamber o p cabinet maintai humidity. water-filled dish. r. , * ., Nkl' 1--Among acceptable sealants- are (/) a 60:40 mixture of microcrystalline wax and refined crystalKire parafitr wax, (2) tissue embedding wax, and (3) a 50:50 mixture ofbeeswax and rosin. at 73 1F (23 0.6)arid 50 2% relative hnmidt 9.1.2 Condition B--Test chamber or desiccator mi tained at 100 IT (38 0.6C) and 90 2% ielatf* humidity. 12. Procet , 12.1 Ph follows: .. ..... i ; ,, 15^ thI2-U F 5 Perm Cups, 10 cm2 an*i25 cm2 ia area, available .from PaulN. Gardner Co., Inc., 316 N.E. First Street, Pompano Beach, FL 330$!, and BYK/Cjardner, Inc., Gardner Laboratory, 2435 Linden Ln,, Silver Spring, l&ID 20910 reive? been found satisfactory for this purpose. ' : top edf 6 Release Paper. Form RP-1K, available; hum the Leneta Go;,' Sli *2.1.2 ii Ho-Ho-Kus, NJ 07423, has been found satisfactory for this purpose. ' 6*1! Spcimen c 7 Paper charts, Form NWK, available from the Leneta Co., have be suitable for this purpose. 30(1 adjust 210 DUP050297393 D 1653 ver possible bstrates, on cedures out- e too brittle 1ms, support d glass cloth >uch support s be smooth n thickness to substrates thods D 823 the coating be methods. The lge for the type i % of the total :ified time and >ns. Permeance mg. 1 position for a 3.5F (23 aterial to be md allow the ional.7 days, amended by tholes or other 0 apply the test ular to the first oats to achieve en in several 'est Methods laterials, the 1 away from , depending .h sides of a at are cured )D between the ormed under t maintained e humidity. :cator main2% relative :o,, P.O. Box pose. . have been fo"00 jO. Procedure 10.1 Prepare at least three perm cups or dishes for each test material as follows: 10.1.1 Fill the cups with desiccant to within 'A in. (6 mm) 0f the top edge. 10.1.2 If the cups are equipped with flanges, place the test specimen between the flanges and adjust the clamps to hold it firmly in position. 10.1.3 If the cups are not equipped with flanges, seal the test specimen to the top edge of the cups with wax as follows: 10.1.3.1 First carefully place the test specimen, cut to the size of the cup, on a thin cardboard ring soaked in molten wax10.1.3.2 Then place the specimen-covered frame over the mouth of the cup. Thoroughly seal the flame to the edge of the cup at the temperature to be used in the test. If the coating is on a substrate or support, place the coated side away from the desiccant in the cup. More 5--Imperfections in the film that are not readily visible, will produce inconsistent results; consequently make sure that the test is always run in triplicate. *" 10.4 Weigh the loaded cups to 1 mg and place them in the lest cabinets or desiccators. Record time, temperature and relative humidity. 10.5 Remove the cups for periodic weighing to determine weight gain. Coatings expected to have high WVT ratings, over 10 perms, may require weighings more frequently than once a day. 10.6 In general, weigh the cups every 24 h for a period of 3 weeks, or until the weight change has become constant. Record the time that weighings are taken to the precision of approximately 1 % of the time span between weighings. Thus, if weighings are made every day, a time to the nearest 15 minutes would be allowed. 10.7 Shake cups containing desiccant everyday to prevent surface saturation of the material If moisture absorbed by the desiccant exceeds 20 % of the desiccant weight, discon tinue the test 10.8 Return the cups to the test chamber immediately after weighing. TEST METHOD it--WET CUP METkOD 11. Test Conditions 11.1 Unless other conditions are agreed upon between the purchaser and the seller, perform the test(s) under one or more of the following conditions: 11.1.1 Condition A--Test chamber or cabinet maintained at 73 1F (23 0.6C) and 50 2% relative humidity. 11.1.2 Condition C--Test chamber or desiccator main tained at 73 1F and very low (near zero) relative humidity. 12. Procedure 2.1 Prepare at least three cups for each test material as follows: 2,1.1 Fill the cups with water to within 'A in. (6 mm) of 12.1.2 If the cups are equipped with flanges, place the test specimen over the opening of the cups between the flanges adjust the clamps to hold them firmly in position. If the coating is on a substrate or support, place the coated side towards the water in the cups. 12.1.3 If the cups are not equipped with flanges, seal the test specimens to the top edge of the cups with wax in accordance with procedures in 10.1.3.1 and 10.1.3.2. 12.2 Weigh the loaded cups to 1 mg and place them in the test chamber. Record time, temperature and relative hu midity, Follow procedures outlined in 10.5 and 10.6. 12.3 Return the cups to the test chamber immediately after weighings. 13. Calculations 13.1 For each material tested, plot the weight change against elapsed time. When a straight line adequately fits the plot of at least four properly spaced points, a nominally steady state exists and the slope of the straight line is the rate of water vapor transmission. 13.2 Calculate one or more of the following, depending on the water vapor transmission characteristics to be determine 13.2.1 Calculate the water vapor transmission rate, WVT: 13.2.1.1 In inch-pound units as follows: WVT = (G/t)/A -- grains per ft2 per 1 h (1) where: G = weight change, grains (from the straight line), t -- time during which G occurred, h, and A = test area, ft2, 1 g = 15.43 grains. 13.2.1.2 In metric units as follows: WVT m (G/t)/A -- grams per m2 per 24 h (2) where: G = weight change, g (from the straight line), t = time during which G occurred, h, and A = test area, m2. 13.2.2 Calculate the permeance, WVP: 13.2.2.1 In inch-pound units as follows: WVP = WVT/4p = grains per ft2 per 1 h per in. of mercury (perms) ' ' where: 4P = S (Hi - R2), S = in. Hg (saturation vapor pressure at test temperature), (see Table 1), Rl = relative humidity at vapor source; and R2 -- relative humidity at vapor sink. 13.2.2.2 In metric units as follows: WVP = WVT/Ap = grams per m2 per 24 h per millimetre (4) of mercury, (metric perms) where: Ap = S (Hj -- Hj), S = mm Hg (saturation vapor pressure at test tempera ture), (see Table 1), i?x = relative humidity at vapor source, and R2 * * relative humidity at vapor sink. 14. Report 14.1 Report the following information: 14.1.1 Method of coating application and curing proce dure used. 211 DUP050297394 D 1653 TABLE 1 Saturation Vapor Pressure Temperature Pressure F 72.3 72.5 72.7 72.9 73.1 73.3 73.4 73.6 73.8 74.0 74.2 74.4 74.5 99.3 99.5 99.7 99.9 100.1 100.2 100.4 100.6 100.8 101.0 101.1 101.3 101.5 c 22.4 22.5 22.6 22.7 22.8 22.9 23.0 23.1 23.2 23.3 23.4 23.5 23.6 37.4 37.5 37.6 37.7 37.8 37.9 38.0 38.1 38.2 38.3 38.4 38.5 38.6 in. Hg 0.800 0.805 0.810 0.816 0.819 0.824 0.829 0.834 0.840 0.845 0.850 0.855 0.860 1.894 1.904 1.914 1.925 1.935 1.946 1.956 1.967 1.978 1.988 1.999 2.010 2.021 mm Hg 20.31$ 20.440 20.565 20.690 20.815 20.941 21.068 21.196 21.324 21.453 21.583 21.714 21.845 48.102' 48.364 48.627 48.891 49.157 49.424 49.692 49.961 50.231 ,, 50.502 ~ 50.774 51.048 51.323 14.1.2 Mean film thickness of the test specimens for each material. 14.1.3 Type of film support used, if any. 14.1.4 Method used (Test Method A (Dry Cup) or Test Method B (Wet Cup)). 14.1.5 Test temperature and relative humidity in the test chamber. 14.1.6 Computed rate of water vapor transmission (WVT), either in inch-pound or in metric units. 14.1.7 The computed permeance in terms of both perms and metric units. 15. Precision and Bias8 15.1 In an interiaboratory study of these test methods in which one operator in each of three laboratories determined in triplicate the permeance of three coatings covering the range of interest for vapor barrier coatings, the interiaboratory standard deviation for the dry-cup procedure was found to be 0.073 perms with 6 df and the interiaboratory wet-cup coefficient of variation 21.54% relative with 6' df, with no results having been discarded. Based upon these values, the following criteria should be used for judging, at the 95 % confidence level, the accept ability of results: 15.1.1 Repeatability: 15.1.1.1 Test Method A--Two results, each the mean of triplicate runs, obtained by the same operator should be considered suspect if they differ by more than 0.25 perms at dry-cup permeance of less than 1.0 perms. 15.1.1.2 Test Method B--Two results, each the mean of triplicate runs, obtained by the same operator should be considered suspect ifthey differ by more than 74.2 % relative at wet-cup permeances of 5 to 30 perms. 15.1.2 Reproducibility--Intralaboratoiy precision is nor mally better than interiaboratory precision. However, one i participant in this exchange has noted relatively large differ ences when the same coating was tested in quadruplicate! with fairly long intervals between tests. 15.2 Bias is not applicable to these test methods. 16. Keywords 16.1 permeability; permeance; perms; water vapor! permeance; water vapor transmission 8 Supporting data are available from ASTM Headquarters. Request i| RR:D! -1064. ' m The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standerd are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technicalcommittee and must be reviewed every five years and ifnot revised, either reapproved orwithdrawn. Your comments are Invited either forrevision of thisstandardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel t/iat your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Race St, Philadelphia, PA 19103. 212 DUP0502 97395 ^ pesignation: D 1654 - 79a (Reapproved 1d84)e1 meihodsdeterminS 0verin&t? atings,8 J* f ad th 3n 21.54% | ^scard^ should ( the accept Standard Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive Environments*1 This standard is issued under the fixed designation D 1654; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year ofiast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovai. This standard has been approved for use by agencies ofthe Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. r Mst' --Editorial changes were made throughout in July 1984. he ean 0f r Should he 2 % relative aon is nor. )wever, one large differ. -ladruplicjk )ds. ater vapor arters. Requts i Scop 11 This method covers the treatment of previously ied or coated specimens for accelerated and.atmospheric lests and their subsequent evaluation in respect to SlrBion, blistering associated with corrosion, loss of adfae^ata scribe mark, or other film failure. 12 This standard may involve hazardous materials, operJoits. wd equipment. This standard does not purport to Ztfre'ss all ofthe safety problems associated with its use. It is T*responsibility ofwhoever uses this standard to consult and mablish appropriate safety and health practices and deter0ge the applicability ofregulatory limitations prior to use. I Referenced Documents 2.1 ASTM Standards: B117 Method of Salt Spray (Fog) Testing2 B 287 Method of Acetic Acid-Salt Spray (Fog) Testing3 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces4 D714 Test Method for Evaluating Degree of Blistering of Paints4 D1014 Test Method for Conducting Exterior Exposure. Tests of Paints on Steel4 D2803 Test Method for Filiform Corrosion Resistance of Organic Coatings on Metal4 3. Significance and Use 3.1 This method provides a means of evaluating and comparing basic corrosion performance, of the substrate, pittreatment, or coating system, or combination thereof, ifter exposure to corrosive environments. i Apparatus ' 41 Scribing Tool--A straight-shank tungsten carbide tip, tohe cutting tool (Brazed tool, Style E, with '/64-in. nose wEus) is recommended; however, other styles may be used I* method is under the jurisdiction of ASTM Committee D-l on Paint and Coatings and Materials and is the direct responsibility of Subcommittee j -7 on Accelerated Tests For Protective Coatings. i (vi""*"' edition approved Nov. 26 and Dec. 3, 1979. Published January 1980. i ; published as D 1654 - 59. Last previous edition D 1654 - 74, >;' | ; ,#<!/ Bock ofASTM Standards, Vols 03.Q2 and 06.01. provided they are ground to a single point having an included angle of 60 15. Any other type of scribing instrument such as a scalpel, razor blade, knife, or sharp pointed tool is unacceptable unless agreed upon between the producer and the user. 4.2 Straightedge--Any straightedge of sufficient length and rigidity to guide the scribing tool in a straight line. 4.3 Air Compressor--A source of compressed air capable of producing 80 psi (550 kPa) open line pressure. 4.4 Air Gun--An air dusting gun and nozzle com bination3 to meet the following specification: Air Consumption, ff/min (m3/min) Pressure, psi (kPa) Nozzle Diameter, in. (mm) 8.4(0.24) 80(550) 0.12(3.0) 4.4.1 A guard consisting of barriers, baffles, or screens is required to protect the operator and other individuals near the area where the air is being used. The guard must be placed between the air nozzle and,the operator. A device such as a sand-blasting cabinet has been found to be acceptable. Nuv' 1:--The use ofan air gun without a guard is in violation of the U. S. Occupational Safety and Health Administration regulation. 4i5 Scraping Tool--A rigid metal spatula, dull knife, or similar instrument. 4.6 Scale--Any rule with l-mm divisions. 4:7 Grid, plastic or wire with l/2-in. (13-mm) squares necessary to permit measurements of the required accuracy. 5. Preliminary Treatment of Test Specimens 5.T Scribed Specimens: 5.1.1 Where specified or agreed upon, prepare each spec imen for testing by scribing it in such a manner that the scribe can be exposed lengthwise when positioned in the test cabinet. This position will allow solution droplets to ran lengthwise along the scribe. 5.1.2 Scribe the specimen by holding the tool at approxi mately a 45 angle to the surface. Position the tool so that only tiie carbide tip is in contact with the surface. Pull the scribing tool to obtain a uniform V-cut through the coating that is being tested. The scribe should be of sufficient length to cover the significant test area but should not contact the 5 Spray gun and nozzles. Model No. 22-L and 0010 have been found satis factory and may be obtained from Spray Systems Co. Equivalents may be used. 213 DUP0502 97396 # D 164 edge of the specimen. The scribe must penetrate all coatings on the metai, leaving a uniformly bright line free of burrs. Quality of the scribe may be observed with the aid of low-power magnification. Note, marie, and describe defects, coding, and flaws that may affect results. 5.1.3 Scribe lines other than those of a single, straight nature may be used if agreed upon between the producer and the user. 5.1.4 Expose scribed specimens in accordance with 6.1 and rate in accordance with Section 7. 5.2 Unscribed Specimens--Specimens coated with paint undercoats, oils, or waxes may be evaluated without a scribe. Expose such specimens in accordance with Section 6 and rate for corrosion of the general surface in accordance with Section 8. 6. Exposure of Test Specimens 6.1 Expose test specimens in accordance with Methods. B 117, B 287, D 1014, D 2803, or any other applicable test method, as agreed upon between the producer and the user. The length of test and evaluation intervals should be agreed upon prior to exposure of specimens. 7. Procedure A--Evaluation of Scribed Specimens 7.1 Method 1 (Air Blow-Off)--Rinse each specimen after completion of the exposure period, using a gentie stream of water at a temperature up to 110T (45C). Holding the nozzle at approximately a 45 angle, blow along the entire scribe line, disturbing the surface adjacent to the scribe mechanically by the air nozzle to ensure an opening for die air blast. Complete the air blasting within 15 min of specimen removal from the exposure cabinet. If the air blasting cannot be completed within the prescribed time, immerse the specimens in water at room temperature dr store in a plastic bag to avoid any drying effect 7.2 Method 2 (Scraping)--Rinse the specimen after com pletion of the exposure period, using a gentle stream ofwater at a temperature up to 110F (45C). Scrape the specimen vigorously with an instrument described in 4.5 while under the gentle stream of the rinse water. Hold the scraper with its face perpendicular to the specimen surface and parallel to the scribe, moving it back and forth across the scribe to remove the coating that has been undercut and has suffered losstof adhesion only, not to remove the coating that still has adhesion. Complete the scraping within 15 min of specimen removal from the exposure cabinet. If scraping cannot be completed within the prescribed time, immerse the speci- TABLE 1 Rating of Failure at Scribe (Procedure A) Representative Mean Creepage From Scribe Millimetres Inches (Approximate) Rating Number OverO Over 0 to 0.5 Over 0.5 to t.0 Over 1.0 to 2.0 Over 2.0 to 3.0 Over 3.0 to 5.0 Over 5.0 to 7.0 Over 7.0 to 10.0 Over 10.0 to 13.0 Over 13.0 to 16.0 Over 16.0 to more 0 OtoVw V&4 to V& V32 to Via Vie to Va * Vb to Via i to V V. to % % to Va 'AtO% % to more 10 9 8 7 6 8 4 3 2 1 0 TABLE 2 Rating of (Inscribed Areas (Procedure B) Area Failed, % Rating Number No failure Otol 2to3,. 4 to 6' ' , 7 to 10* - nto2a 21 to 30 31 to 40 41 to 55 56 to 75 Over 75 ia 9 87 6 5 4 3 2 1 0 mens in water at room temperature or store in a plastic bag to avoid any drying effect. Nwx' 2--Some specimens exposed to natural weathering do not requite rinsing, air blasting, or scraping to evaluate corrosion. Alterna tive methods may be used ifagreed upon between the producer and the user.. 7.3 Rating--Rate the corrosion or loss of paint extending from a scribe mark as prescribed in Table l. Record the representative mean, maxipium, and minimum creepage from the scribe, and note whether or not the maximum is an isolated spot. Also, rate in accordance with Table 2 the prevalence of corrosion on areas removed from the scribe. 8, Procedure B--Evaluation of Unscribed Areas 8.1 Rinse the specimen after completion of the exposure period (Section 6), using a gentle stream of water at a temperature up to 100T (40*C). Dry the. jsurface of the specimen with paper towels or compressed air. Drying should be done in such a manner that the corrosion on the specimen surface is not disturbed. 8.2 Evaluate unscribed specimens for corrosion spots, blisters, and any other types of failure that may occur. Depending upon the contour of the specimen, the use of a grid,'as described'in 4.7, is recommended as an aid in evaluating this type failure (Fig. 1). The percent of surface failure^ excluding rust staining or run down, can be esti mated by counting the number of squares that have points of failure and relating this number to the total number of squares covering the test area. Discount corrosion within Vi in. (12.7 mm) of edges. 8.3 Rating--Convert percent failure to th'e rating number in accordance with Table 2. In some instances, the rating number may be used as a factor with the corresponding exposure time intervals to produce a-performance index number. ' T ' Nwx' 3--Formation of under-film corrosion may be evaluated and reported in accordance with Table 2 if the film is first carefully stripped with a neutral stripper.. Exercise care-to avoid alteration ofthe corrosioa pattern or pretreatment., ;. f j Nyz' 4--Where the' character of & failure permits, the photo* graphic blister standards given in Test Method D 714 may be used to describe the results of the exposure test, in respect to size of blistersor corroded areas, white Method- D 610 may serve to describe the' foquency and distribution, <if desired. i ; : 9. Report 9.1 Report the ratings of the test specimens, the proce dures, and, for scribed panels, the method followed. Alsft ; No- repo; subje 10. i 10 meas DUP050297397 D 1654 <r 12 > :ic. do not Yltemaand the :nding: rd the iepage a is an 2 the ribe. aosure at a of the drying on the spots, occur, e of a aid in urface e esti:ntsof er of in Vi mber ating ading index ;ed and tripped erosion photoused to sters or the fre- k 8)i"- N{|' --11n. = 25.4 mm. FIG. 1 Typical Grid with Va-fn. (13-mm) Squares report the exposure test to which the specimens were subjected. 10. Precision and Use 10.1 Since this is a method of evaluation based on measurements after various tests, the statement of precision applicable to each specific method of exposure to corrosive atmospheres applies. The preferred methods of measure ment, using ruled plastic sheets, are at least equal in precision to the various methods of exposing test specimens to corrosive environments. The American Society for Testing and Materials takas no position respecting the validity ofany patentrights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnotrevised, eitherreapproved or withdrawn. Yourcomments are Invitedeither hrrevision of this standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. H you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. proceAlso, DUP050297398 ijOlM Designation: D 1730 -- 67 (Reapproved 1984)e1 dizing action, Standard Practices for Preparation of Aluminum and Aluminum-Alloy Surfaces for crystal! to inhi bility i Painting1 produc carried This standard is issued under the fixed designation D 1730; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year oflast reapprovaL A superscript epsilon () indicates an editorial change since the last revirion or reapprovaL minunr immer to 140` 61 N}~' --Section 2 was added and subsequent sections were renumbered editorially in September 1984. 2 min N' 6, and 7 1. Scope 1.1 These practices cover four types of treatment for preparation of aluminum and aluminum-alloy surfaces for painting, as follows: 1.1.1 Type A--Solvent Cleaning. 1.1.2 Type B--Chemical Treatments. 1.1.3 TypeC--Anodic Treatments. 1.1.4 Type D--Mechanical Treatments. These four types cover a number of procedures, as described herein. 1.2 Variations in surface treatment produce end condi tions which differ, and which do not necessarily yield identical results when paints are applied. Service conditions will dictate the type of surface preparation that should be selected, although the quality produced by any individual method may vary with different alloys. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability ofregulatory limitations prior to use. 3.1.3 Method 3, Vapor Degreasing, in special equipment employing trichloroethylene vapor, in accordance with Method A, Procedure 2 of Method D 609. 4. Type B--Chemical Treatments .. N' 1--Materials and procedures employed in these methods of ~ treatment are available from a number of sources as proprietary compounds or methods. Selection may be made from available sources, 4.1 Method l. Alkaline Cleaners--Alkaline solutions, such as caustic soda, etch the metal, thus destroying the natural oxide film. They are followed by an acid treatment, preferably nitric acid or phosphoric add. They shall not be used on assembled structures. Inhibited alkaline cleaners are sometimes employed as a pretreatment to remove grease and oil prior to an add treatment. Inhibited alkaline cleaners do not etch the surface. They are not generally recommended unless followed by a conversion treatment, such as described in Methods 4, 5, 6, or 7. 4.2 Method 2, Sulfuric Acid, Chromium Trioxide Etch--. This treatment provides a clean and uniform surface without undue etching, and is effective for removing oil and water or othei Method N' Federal 4.5 . process warm prising trioxidi conver green t alloy t adhere: is recoi service, carried treatmt from 3( 3 and i N' of Type MIL-C-i 2. Referenced Document stains and any film formed during heat-treatment The etching solution is prepared by adding 1 gal (3.7S L) of 4.6 v process 2.1 ASTM Standard: concentrated sulfuric add and 45 oz (1.28 kg) of chromium ss'Q) D 609 Methods for Preparation of Steel Panels for Testing trioxide to 9 gal (34 L) ofwater. It is used at a temperature of chrom: Paint, Varnish, Lacquer, and Related Products21 160 to 180'F (71 to 82C) (depending on the alloy and the amount of film) for about 5 min and is followed by a water rinse.' potassi 3. Type A--Solvent Gearing rinse. This treatment produces a passive surface suitable for The trt 3.1 Solvent cleaning does not disturb the natural oxide painting under mild to intermediate exposure conditions and on the film on the metal and may prove adequate for some where clear finishes are to be applied. metal i applications, such as ambient indoor or very mild service 4.3 Method 3, Alcoholic Phosphoric Acid Cleaner--This mende< conditions. Three methods may be employed, as follows: treatment involves the use of an aqueous solution of and for 3.1.1 Method 1, Manual Swabbing or Dip- Washing, with phosphoric acid (10 to 15 volume %) with alcohol or other 4.7 / a solvent such as mineral spirits or high-flask solvent organic solvents, together with wetting agents, emulsifying process naphtha. With this method it is extremely difficult to prevent agents, etc. The solution may be applied by swabbing or aqueou accumulation ofcontaminants on the swab or in the solvent. dipping at room temperature (70 to 90F (21 to 32C)), and accelen This method is only recommended when other treatments should be allowed to remain on the surface for several The alt are impractical. minutes, followed by thorough rinsing with clean water. A phous, 3.1.2 Method 2, Solvent Spray Cleaning, in accordance very thin phosphate film is formed which tends to protect the light-br 1 with Method A, Procedure 1 of Methods D 609. metal and promote paint adhesion under mild to intense2 diate exposure conditions. and the This ms s 1 These practices are under the jurisdiction of ASTM Committee B-8 on Metallic and Inorganic Coatings. i I Current edition approved Sept. 8,1967. Published November 1967. Originally published as D 1730-60. Last previous edition D 1730-66. 2 Annual Book ofASTM Standards, Vol 06.01. N' 2---U.S. Military Specification MIL-M-10578B describe* * treatment of this type, 4.4 Method 4, Crystalline Phosphate Treatment--This surface-coating method consists in reacting the aluminum conditk Process applicai in from 4.8 A surface in a zinc-acid-phosphate solution containing on- 6)--Thi 216 DUPO 50297399 uipment ice with lettods of >rofirietary le sources. olutions, ying the eatment, 11 not be aners are ease and :aners do imended described e Etch-- : without nd water ;nt The 78 L) of iromium nature of and the a water able for ons and r--This ution of or other lulsifying ibbing or C, and r several water. A rotect the interme- lescribes a mt~--This luminuna ning oxi- D 1730 Sizing agents and other salts for accelerating the coating action. The aluminum surface is converted to a finely crystalline, phosphate coating of the proper texture adapted [0 inhibit corrosion and increase the adherence and dura bility of any applied paint film. It is recommended for product finishes. The phosphate coating process may be carried out by immersion or spray application. The alu minum surface is converted to the phosphate coating by immersion in the processing solution for 30 s to 4 min at 125 to HOT (51 to 60C), or by spraying the solution for 10 s to 2 min at 125 to 160F (51 to 71C). N' 3--Before applying the treatments according to Methods 4, 5, (, and 7 ofType B, the aluminum surfaces should be freed ofgrease, oil, or other foreign material by means of the procedure described in jdethod 3 ofType A, Method 1 ofType B, or any other suitable method. N' 4--This treatment complies with the requirements of U.S. federal Specification TT-C-490. 4.5 Method 5, Amorphous Phosphate Treatment--This process comprises treatment of clean aluminum surfaces in a warm (95 to DOT (35 to 54C)) aqueous solution com prising phosphoric, and hydrofluoric acids, chromium trioxide or a solution thereof. The aluminum surface is converted to a thin, adherent, amorphous coating, iridescent green to gray-green in color, depending upon the aluminum alloy treated, which inhibits corrosion and increases the adherence and durability ofapplied paint films. This method is recommended for use under the more severe conditions of service, and for product finishes. The coating process may be carried out by immersion or spray application. The time of treatment will vary from 15 to 45 s for the spray process, and from 30 s to 3 min for the immersion application (see Notes 3 and 5). N' 5--Most of the treatments conforming to Methods 5, 6, and 7 ofType B comply with the requirements of U. S. Military Specification M1L-C-5541. 4.6 Method 6, Carbonate Chromate Treatment--This process comprises treatment in a hot (180 to 190"F (82 to 88C)) dilute solution of sodium carbonate and potassium chromate for periods from 2 to 20 min, followed by a water rinse. The surface is then given a final treatment in hot 5% potassium dichromate solution, followed by a final rinse. The treatment produces a thin, adherent, conversion coating on the surface, increasing the corrosion resistance of the metal and promoting paint adhesion. This method is recom mended for use under the more severe conditions of service and for product finishes (see Notes 3 and 5). 4.7 Method 7. Amorphous Chromate Treatment--This process comprises treatment of clean aluminum surfaces in aqueous chromium trioxide solutions containing suitable accelerating agents such as fluoride-containing materials. The aluminum surface is converted to an adherent, amor phous, mixed metallic oxide coating, irridescent golden to light-brown in color, which increases the corrosion-resistance and the adherence and durability of any applied paint film. This method is recommended for use under the more severe conditions of service and for product finishes. The coating Process may be carried out by immersion, spray, or brush application, at room temperature (70 to 90F (21 to 32C)), in from 15 s to 5 min contact time (see Notes 3 and 5). 4.8 Method 8, Acid-Bound Resinous Treatment (see Note 6)--This surface treatment involves the use of a suitably applied add-bound resinous film of approximately 0.3 to 0.5 mils (7.6 to 12.7 pm) thickness. The treatment is based on three primary components: a hydroxyl-containing resin; a pigment capable of reacting with the resin and an acid; and an acid capable of insolubilizing the resin by reacting with the resin, the pigment, and the metal substrate. The alu minum surface should be prepared by Methods 1, 2, or 3 of Type A (see Section 3) or chemical treatments. Type B, 4.1 or 4.2 prior to the application of this treatment. The film may be applied by brush, spray, or dip. Under normal conditions it should dry sufficiently for recoating within 30 min; and within 8 h it should not be softened by organic solvents commonly used in paint coatings. The film has good adhesion to the metal substrate and promotes good adhesion of most subsequent organic coatings to itself. This method is recommended for severe service conditions, particularly on fabricated structures, either in the shop or in the field. N' 6--^Materials meeting the requirements of U.S. Military Spec ification MIL-P-15328b may be used to apply Method 8 of Type B. 5. Type C--Anodic Treatments (see Note 7) 5.1 Anodic treatment in either sulfuric acid or chromium trioxide electrolyte will provide a protective and inert oxide coating which increases the corrosion-resistance of the metal and promotes paint adhesion. It is recommended where maximum corrosion-resistance by the treatment itself is desired. Anodic treatments should not be used on assemblies of dissimilar metals. The two procedures are as follows: N' 7--Treatments conforming to Methods i and 2 of Type C comply with the requirements of U.S. Military Specification MIL A-8625. 5.2 Method I, Sulfuric Acid Anodic--This treatment con sists in making the part the anode in a 15% sulfuric acid electrolyte (by weight) and applying current at a potential of about 16 to 18 V and a current density of 12 A/ft2 until desired thickness of coating is obtained. After rinsing in cold water, the coating is sealed for 10 min by treatment in a boiling solution of 5% potassium dichromate. This method is not recommended where danger of acid entrapment is encountered. 5.3 Method 2, Chromium Trioxide Anodic--This treat ment consists in making the part the anode in a 10 weight % chromium trioxide electrolyte at a temperature of 100*F (38C) and applying a potential of40 V for a period of 30 to 60 min. After first rinsing in cold water, the coating is finally rinsed in water at 150F (66C) minimum, and dried; an optional final sealing treatment to obtain maximum protec tion is obtained by immersion in a solution containing 0.01 g chromium trioxide per litre of water (0.0013 or 1 gal) at a temperature of 208 to 212F (98 to 100) for 5 min. 6. Type D--Mechanical Treatments 6.1 Method 1, Hand or Power Wire-Brushing, or other abrasive treatment. Wire-brushing, either by hand or power, roughens the surface of the metal and mechanically im proves the anchorage for superimposed paint films. The disadvantages are that the natural Oxide film on the metal is disrupted and oil or grease films and other foreign matter are not completely removed. 217 DU P0502 97400 r # D 1730 6.2 Method 2, Sandblasting, where employed on. aluminum or its alloys, must be carried out at relatively low pressures and with a fine silica sand. It roughens the surface and mechanically improves the anchorage for paint films, but destroys the natural oxide film on the metal. Where used, it should be followed by an inhibitive chemical treatment. The American Society for Testing amt Materials takes noposition respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or tor additionalstandards and should be addressed to ASTM Headquarters. Ycuc comments will receive careful consideration at a meeting of die responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. h r 1. s i. k tion l,: atm addi ther- ' estajt milk 2.B 2n ' j vfi. Ji`l 3. T 3.1 folio' 3.'l 3.1 is Sectii cond ident will selec 4. S 4. ' r the r 4.1 solve It is t this n ,|S the s prepa ; ; 4.3 Vf ! Meth i 4.4 ;if ! accor | of M 218 DUP050297401 |jj^ Designation: D 1731 - 67 (Reapproved 1984)61 Standard Practices for Preparation of Hot-Dip Aluminum Surfaces for Painting1 This standard is issued under the fixed designation D 1731; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. ** N' --Section 2 was added and subsequent sections were renumbered editorially in September 1984. 1. Scope 1.1 These practices describe procedures for the prepara tion of hot-dip aluminum surfaces for painting. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter-:, mine the applicability of regulatory limitations prior to use. 2. Referenced Document ethylene vapor. Solvent cleaning does not disturb the natural oxide film on the metal and may prove adequate for some applications. 5. Chemical Treatment 5.1 The surfaces may be prepared for painting by any of the methods for chemical treatment (Note 1) described in 5.2 to 5.9: N' 1--Materials and procedures employed in these methods of treatment are' available from a number of sources as proprietary compounds or methods. Selection may be made from available sources. 2.1 ASTM Standard: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 3. Types of Surface Preparations 3.1 Two types of surface preparations are covered as follows: 3.1.1 Solvent Cleaning, and 3.1.2 Chemical Treatments. 3.2 These two types cover several methods as described in Section 5. Variations in surface treatment produce epd conditions which differ and which do not necessarily yield identical results when paints are applied. Service conditions will dictate the type of surface preparation that should be selected. 4. Solvent Cleaning 4.1 The surfaces may be prepared for painting by any of; the methods for solvent cleaning described in 4.2 and-4.3. , ' 4.2 Method 1--Manual swabbing or dip washing with a solvent such as mineral spirits or high flask solvent naphtha. It is extremely difficult to produce a clean metal surface by this method. Accumulated contaminants in the solvent or on the swab are frequently redeposited on the surface being prepared. 4.3 Method 2--Solvent spray cleaning in accordance with Method A, Procedure 1 of Methods D 609. 4.4 Method 3--Vapor degreasing in special equipment in accordance with the latest revision of Method A, Procedure 2 of Method D 609, employing trichlorethylene or perchlor- 5.2 Method 1, Alkaline Cleaners--Etching alkaline solu-. tions, such as caustic soda, should be avoided because of the possibility of dissolving away the aluminum coating thereby exposing the base metal. Since inhibited alkaline cleaners do not etch the surface, they can be used to remove grease, oil, and other organic solids from hot dip aluminum. After alkali cleaning, the surface should be thoroughly rinsed with clean water. Most often alkaline-cleaned surfaces are subsequently processed by one of the following methods, described in 5.3 to 5.9: - 5.3 Method 2, Alcoholic Phosphoric Acid Cleaners--This treatment involves the use of an aqueous solution of phosphoric acid with alcohol or other organic solvents, together with' wetting agents, emulsifying agents, etc. The solution may be applied by swabbing or dipping (preferably at a temperature of 70 to 90F (21 to 32C)). The solution should remain on the surface for several minutes, followed by thorough rinsing with clean water. A very thin phosphate film is formed which tends to protect the metal and promote paint adhesion. N' 2--Materials meeting the requirements of the latest revision of U.S. Military Specification MIL-M-10578B may be used. 5.4 Method 3, Acid Fluoride Deoxidizer--This treatment includes the use of nitric or sulfuric acid with chromium trioxide and a fluoride. It provides a clean and uniform surface without undue roughening and is effective for removing inorganic soils and any film formed during the production of the hot dip aluminum. The deoxidizing solution is generally used at a temperature of 70 to 130*F (21 to 54C) (depending on the alloy and the amount of film) and is followed by a water rinse. 1 These practices are under the jurisdiction of ASTM Committee B-8 on Metallic and Inorganic Coatings. Current edition approved Sept. 8, 1967. Published November 1967. Originally Published asD 1781-60. Last previous edition D 1731-66. 2 Annuat Book ofASTM Standards, Vol 06.01. N' 3--Before applying the treatments according to Chemical Treatment Methods 3, 4, S, 6 and 7, the aluminum surfaces should be Seed of grease, oil or other foreign material by means of the procedure described in Solvent Cleaning Method 3, Chemical Treatment Method 1 or any other suitable method. 2\9 DUP0502 97402 f' D 1731 5.5 Method 4, Crystalline Phosphate Treatment--This surface-coating method consists in reacting the aluminum surface in a 130 to 145F (54 to 63C) (approximately) zinc acid-phosphate solution containing oxidizing agents and other salts for accelerating the coating action. The aluminum surface is converted to a crystalline, phosphate coating of the proper texture adapted to inhibit corrosion and increase the adherence and durability of any applied paint film. The phosphate coating process may be carried out by immersion or spray application. The aluminum surface is converted to the phosphate coating by immersion in the processing solution for 30 s to 4 min, or by spraying the solution for 10 s to 2 min (Note 3). 5.6 Method 5, Amorphous Phosphate Treatment (see Note 4)--This process comprises treatment of clean aluminum surfaces in a 90 to I25T (32 to 5TC) aqueous solution comprising phosphoric, hydrofluoric acids and chromium trioxide. The aluminum surface is converted to a thin, adherent, amorphous coating, iridescent green to gray green in color, depending upon the aluminum alloy treated, which inhibits corrosion and increases the adherence and durability of applied paint films. The coating process may be carried out by immersion or spray application. The time of treat ment will vary from 15 to 45 s for the spray process and 30 s to 3 min for the immersion application (Note 3). 5.7 Method 6, Carbonate Chromate Treatment (see Note 4)--This process comprises treatment in a 160 to 180T (71 to 82C) dilute solution of sodium carbonate and potassium chromate for periods from 2 to 20 min, followed by a water rinse. The surface is then given a final treatment in a 150 to 160F (66 to 71C), 5% potassium dichromate solution followed by a final rinse. The treatment produces a thin, adherent, conversion coating on the surface, increasing the corrosion resistance of the metal and promoting paint adhesion (Note 3). 5.8 Method 7, Amorphous Chromate Treatment (see Note 4) --This process comprises treatment of clean aluminum surfaces in aqueous chromium trioxide solutions containing suitable accelerating agents such as fluoride-containing ma terials. The aluminum surface is converted to an adherent, amorphous, mixed metallic oxide coating, iridescent golden to light brown in color, which increases the corrosion resistance and the adherence and durability of any applied paint film. The coating process may be carried out by immersion, spray or brush application, at 70 to 130F (21 to 54C), in from 15 s to 5 min contact time. It may be necessary to precede this treatment with a deoxidizer as described in Method 3 (see Note 3). N' 4--Most ofthe treatments conforming to Chemical Treatment Methods 5,6, and 7, comply with the requirements ofthe latest revision of U.S. Military Specification MIL-C-5541. 5.9 Method 8, Acid-Bound Resinous Treatment (see Note 5) --This surface treatment is based on the deposition of an acid-bound resinous film of approximately 0.3 to 0.5 mils .. (7.6 to 12.7 jtm) in thickness on the aluminum surface in such a manner as to enhance the adhesion of subsequently applied paint coatings. The treatment is based on three primary components: a hydroxyl-containing resin; a pigment capable of reacting with the resin and an add; and an add capable of insolubilizing the resin by reacting with the resin, the pigment and the metal substrate. The aluminum surface should be pretreated by Solvent Cleaning Methods 1, 2 or 3 or Chemical Treatment Methods 1 or 2 prior to the application of this treatment. The film may be applied by brush, spray, or dip. Under normal conditions it shall dry suffidently for recoating within 30 min; The film has good adhesion to the metal substrate and promotes good adhesion of most subsequent organic coatings to itself. N' 5--Materials meeting the requirements ofthe latest revision of U.S. Military Specification MJL-C-15328 may be used to apply to Chemical Treatment Method 8. The American Society for Testing amt Materials takes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standardis subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments are Invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive csreful consideration as a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should mate your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. Set 1.1 prepai follow Cla. Treatn In gen the tw cleanir resultii liminai mildly corrosimany t the abc N' frequent without suitable j fixed tin coatings example consisten remove 5 taminatk in. (25 ju 1.2 ; ations, address the resp establisi mine th (See No 2. Proce 2,1 a conversic magnesii `These j Metallic and Current ei Published as z For inft Specification *ion on A Standards, V "onferrous f 220 DUP050297403 see Note iminuro ntaining ling madbenent, t golden oitosion applied out by 'F|21 to may be dizer as Treatment it revision see Note m of an 0.5 mils rface in squently in three pigment an acid se resin, ; surface 4 2 or 3 to the plied by hall dry as good dhesion jvision of apply to Designation: D 1732 - 67 (Reapproved 1984) Standard Practices for Preparation of Magnesium Alloy Surfaces for Painting1 This standard is issued under the fixed designation D 1732; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. These recommended practices have been approvedfor use by agencies ofthe Department ofDefense andfor listing in the DoD Index ofSpecifications and Standards. j. Scope 1.1 These practices cover two classes of treatment for preparation of magnesium alloy surfaces for painting, as follows: Class I--Chemical Treatments. Treatments. Class U--Anodic In general, the latter treatments are the more protective_ of the two classes. Mechanical (abrasive) treatments, solvent cleaning, alkaline solution treatments, and acid pickles not resulting in protective conversion coatings are suitable pre liminary treatments only for metal to be exposed under mildly corrosive (indoor) exposures. When a high degree of corrosion protection and paint adhesion are desired, as in many outdoor environments, surface preparation by one of the above conversion-coat classes is necessary. N ' 1--Testing of Coatings--Quality control tests of coatings are frequently desirable, and these generally consist of exposures, with or without paint, to salt spray, humidity, or natural environments, with suitable procedures for assessing the degree of breakdown suffered after fixed time intervals. It is recommended that quality control tests of coatings shall be made as far as possible with high-purity material (for example AZ31A alloy),21the inherent corrosion rate ofwhich is relatively consistent from batch to batch) and that precautions shall be taken to remove surface contamination before coatings are applied. Such con tamination shall be removed by acid pickling to a depth ofat least 0.001 in. (25 pm) per side. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. (See Note 11.) PRELIMINARY TREATMENT OF SURFACES 2. Procedure 2.1 Certain anodic treatments simultaneously produce conversion coatings on, and remove contamination from, magnesium alloy surfaces. In general, however, apply con 1 These practices are under the jurisdiction of ASTM Committee B-B on Metallic and Inorganic Coatings. Current edition approved Sept. 8, 1967. Published November 1967. Originally published as D 1732-60. Last previous edition D 1732-66. 2 For information concerning magnesium and aluminum alloys, see ASTM Specification B 80, B 90, B 91, B 93, B 107, and B 209 covering these alloys, In the section on Aluminum and Magnesium and Their Alloys, Annual Book ofASTM Standards, Vol 02.02. See also ASTM Practice B 275, for Codification of Certain Nonferrous Metals and Alloys, Cast and Wrought. version coatings only to surfaces previously freed from all contamination, including oxide, rolling-scale, corrosion product, bumed-on drawing and forming lubricant, and the contamination introduced by blast cleaning and fabrication operations. Contamination in or under surface conversion coatings seriously reduces their protective values (Note 2). For the removal oftenacious surface contamination, such as rolling-scale or casting skin, an acid pickle to dissolve some of the actual surface is essential. When organic contamina tion, such as grease or oil, is also present, an initial degreasing operation in solvent or in an alkaline degreasing solution is usually necessary to allow the subsequent acid to wet the surface. These matters are discussed in more detail under the headings of the specific cleaners or treatments (Note 3), as follows: 2.2 Alkaline Cleaners--Oil, grease, and old (but not baked) chrome-pickle coatings are readily removed by most commercially available heavy-duty alkaline cleaners; but such cleaners are not suitable for removing oxide and the like, for which purpose use acid pickles, preceded by alkaline cleaners. Remove graphite lubricant and also baked chromepickle coatings by a solution conforming to the following composition: Caustic soda (NaOH) Wetting agent Water (Note 4) 12oz(90g) 0.1 oz (0.74 g) I gal (1 litre) Soak the parts in the above cleaner for 10 to 20 min at boiling-point, and a treatment shall follow either in the chromic acid-nitrate pickle described under 2.3.3 or, for parts machined to fine tolerances, in the chromium trioxide solution described under 2.3.1. After alkaline cleaning, rinse in water very thoroughly. Alkaline cleaners may be held in plain steel tanks. 2.3 Acid Cleaners (Note 1)--Acid picking removes millscale, oxide, corrosion product, and the like. Use as a preliminary treatment for surface conversion coatings when the highest degrees of surface uniformity and protective values are required. Add cleaners are as follows: 2.3.1 For Sand and Permanent Mold Castings: 2.3.1.1 Nitm-Sulfuric Acid Solution--Use a solution of 8 volume % of concentrated nitric acid (HNOa) plus 2 volume % Of concentrated sulfuric add (H2S04) in water (see Note 1(a)) at 70 to 90F (21 to 32"C) as a preliminary treatment for new sand tastings arid to remove the surface contaminating effects of blast cleaning. Immerse for about 10 to 15 s, or until 0.002 in. (51 urn) per surface is removed. The solution may be held in ceramic, rubber, synthetic rubber, or vinyl-lined tanks. 221 DUP050297404 D 1732 2.3.1.2 Chromic Acid Solution--Use a boiling 20 weight % solution of chromic anhydride (0rO3) in water to remove old chemical and anodic treatments, corrosion product, and oxide layers, without significant dissolution of metal and hence without changing the dimensions of ma chined parts. Immersion time varies from I to 5 min, depending upon the condition of the surface. The solution may be held in lead-lined steel or ASTM alloy No. 990A or its Aluminum Association equivalent, alloy No. 1100 alu minum tanks. 2.3.2 For Die Castings: 2.3.2.1 Chromium Trioxide-Nitric-Hydrofluoric Acid So- lution--This solution is used to produce a smut-free surface on die castings, without violent attack of the metal. The solution shall conform to the following composition: Chromium trioxide (Cr03) Hydrofluoric add (60% HF) Nitric acid (70% HN03) Water (Note 4) 37.5 oz (280 g) 1 ft oz (8 ml) 3.25 ft oz (25 ml) to 1 gal (1 litre) Immerse the parts in the above solution at 70 to 90F (21 to 32C) for 30 s to 2 min, or until a bright, clean surface is obtained. The solution may be held in tanks lined with synthetic rubber or vinyl-base materials. 2.3.3 For Wrought Products: 2.3.3.1 Acetic Acid-Nitrate Solution--This solution rap idly removes surface contamination to 0.001 in. (25.4 pm). Use for wrought parts subsequently to be finished for the maximum protective value. The solution shall conform to the following composition: Glacial acetic acid Sodium (NaNCy Water (Note 4) 25.5 fl oz(199 ml) 6.6 oz (49.5 g) to 1 gal (1 litre) Immerse the parts in the above solution at 70 to 90F (21 to 32C) for 30 s upwards, or until a bright, clean surface is obtained. When heavy surface contamination, such as hot rolled mill-scale is to be removed, immersion times shall be sufficient to remove at least 0.001 in. (25 pm) per surface. The solution may be held in No. 990A aluminum, ceramic, or rubber-lined tanks. 2.3.3.2 Chromium Trioxide-Nitrate Solution--Use this solution following the use of the method described in 2.2 for the removal of bumed-on graphite lubricants from hotformed parts. The solution shall conform to the following composition: Chromium trioxide (Ct03) Sodium nitrate (NaN03) Water (Note 4) 1.5 lb (180 g) 2 oz {15 g) to 1 gal (1 litre) Immerse the parts in the above solution at 70 to 90F (21 to 32C) for approximately 5 min, for the removal of graphite. 2.4 Abnormally slow reaction in the above solution indi cates that it is depleted and that the pH has risen to 1.7 or higher. Revivify the solution by the addition of chromium trioxide to bring the pH back to 0.5 to O.7. Attempt no more than four revivifications. The solution may be held in ceramic, No. 990A aluminum, 18-8 stainless steel, or syn thetic rubber-lined tanks. N' 2--Removal of Contamination by Welding Fluxes--When a part to be painted has been welded by an operation involving the use of flux,-such flux shall be removed before the subjection ofthe part to any surface preparation process. Such removal shall be made imniediately by immersing the part in hot water with scrubbing, and finally by immersing it for 1 b in a boiling 5% solution of sodium dichromate, after which the part shall be well rinsed. N' 3: Suspension of Articles for Treatment--The use of magne sium alloy suspension wires is preferred for use in add pickles in order to avoid objectionable contamination of the solutions through dissolu tion of the wire materials. Heavy metal contamination, particularly of copper, may deposit on the magnesium surface and lead to seriously reduced corrosion resistance. Copper suspension wires in the hot dicbromate solutions are not objectionable. N' 4: Quality of Water--In the preparation and make-up of acid pickles, dichromate solutions, and hot-water rinses, precautions shall be taken against the use of water contaminated with heavy-metal impuri ties, or excessive chlorides or sulfates. No upper limits can be specified at this stage for soluble impurities in the water, but powdering of coatings and poor resistance to corrosion are known to result from the use of contaminated water. Thus, when a choice exists, water from steam condensate or ion-exchange-treated water shall be employed in prefer ence to well water or hard tap water. SURFACE PREPARATION PROCEDURES--CHEMICAL 3. Class I, Type I (Chrome Pickle)3 3.1 Scope--Class I, Type I treatment is applicable to all formsrand alloys of magnesium except certain special alloys containing silver, but since it may remove as much as 0.0006 in. (15 pm) of metal per surface, it shall not be used on parts machined to fine tolerances. When properly applied, the process constitutes a good paint base, but rigid control is required at each step. The treatment is applicable to magne sium alloy containing inserts of, or attached to, other metals. 3.2 Procedure--For wrought parts the bath shall conform to the following composition: Sodium dichromate (Na2Cr207-2H20) Nitric acid (HN03) (sp gr 1.42) Water (Note 4) 1.5 lb (180 g) 1.5 pt (187 ml) to 1 gal (1 litre) 3.2.1 For die-, sand- and permanent-mold castings the solution shall conform to the following composition: Sodium dichromate (Na2Cr307 2H20) Nitric acid (HN03) (sp gr 1.42) SodiUm potassium, or ammonium acid fluoride (NaHFj, KHF3, or NH4HF2) Water1(Note 4) 1.5 lb (180 g) 1.5 pt (187 ml) 2oz(15g) to 1 gal (1.0 litres) For wrought products, sand, and permanent-mold castings the above solutions operate at 70 to 90F (21 to 32C). The immersion times shall be from 1 to 2 min, the necessary time increasing with use of the solution. For die-castings give the parts a 15 to 30 s dip in water at 160 to 180F (71 to 82Q, followed immediately by a 10-s dip in the second of the above baths, operated at 120 to 140F (49 to 60Q. Failure to preheat the castings results in no coating in 10 s. 3.2.2 Following immersion remove the parts, allow to drain for not less than 5 s nor more than 30 s, then wash thoroughly in cold running water, followed by a dip in hot water at 160 to 180"F (71 to 82C) to facilitate drying. Do not allow the parts to drain following the chromate treatment for more than the specified 30 s; excessive drainage times result in powdery coatings of poor value as paint bases. Such coatings also result from the use of hot-water rinses, the temperatures of which are in excess of 180F (82*Q. Paint the parts preferably immediately after they are dry. The solution may be held in Type 316 stainless steel, or ceramic tanks or in steel tanks lined with synthetic rubber or 3 Conforming to Class I, Type I treatments are the Dow No. I process, the AMC "A" process, and the Type 1 process of Military Specification MIL-M-3171A 222 vinyl-base m: Aluminum minum are pickle. 3.3 Revivij metal, associ cates that tht plished by tht the dichionu free nitric ad when the free 0.5 pt/gal (6 procedure) -a ZK60A alloy if good paintsolution or lustrous coat for the best Revivify in a Revivificat Number 1 2 3 to 6 4. Class 1,7 4.1 Scopetypes and fo the limitatio essentially th In protective somewhat su severe expos 4.2 Procet under Sectio immediately lowing comj Sodium dichrom Calcium or magi Water (Note 4) Boil the par rinse them i water at a more than I the paint ct solution ma N' 5: G. intended to pi arising in the coatings: (a) Spotted-< or by the prese to or during tfc (b) Nonadhi U) Too k and rinsing, (2) Ratio (2) Temp (4) Metal (5) Solutl DUP050297405 magnein order dissoluilarly of eriously the hot of acid shall be irnpuricifiedat coatings J use of < steam i prefer- : to all . alloys 0.0006 n parts :d, the itrol is nagnemetals. inform iv to wash t hot > not it for esult Such , the Paint The amic ;r or ' D 1732 vinyl-base materials. Tanks of ASTM alloy No. 990 A, or its /Vluminum Association equivalent, Alloy No. 1100 alu minum are satisfactory for the nonfluoride-containing pickle. 3.3 Revivification ofSolutions--Sluggish reaction with the metal, associated with pale yellow, lustrous coatings, indi cates that the solution is depleted. Revivification is accom plished by the addition ofdichromate and nitric acid, to raise tbe dichromate again to 1.5 lb (180 g)/gal (1 litre) and the free nitric acid to levels indicated in the table below. Revivify when the free nitric acid content of the solution is depleted to 0.5 pt/gal (62.3 ml/1 litre) (see Section 11 for analytical procedure) and shall take place once only for Ml and ZK60A alloys,3 and not more than six times for other alloys ifgood paint-base properties are desired. Excessive use of the solution or too many revivifications result in smooth, lustrous coatings not possessing the degree of etch necessary for the best paint adhesion with conventional primers. Revivify in accordance with the following table: Revivification Number Adjust Concentration ofHN03to: 1 2 3 to 6 1.3 pt/gal (162 ml/1 litre) f. I pt/gal (137 ml/1 litre) 0.9 pt/gal (113 ml/1 litre) 4. Class I, Type II (Sealed Chrome Pickle)4 5 * 4.1 Scope--Class I, Type II treatment is applicable to all types and forms of magnesium-base alloys, subject only to the limitations of the Class I, Type I treatment, since it is essentially the same process as the latter, followed by sealing. In protective qualities and as a paint base, this treatment is somewhat superior to that of Class I, Type I treatment under severe exposure conditions (Note 5). 4.2 Procedure--Following chrome pickling as specified under Section 3 and rinsing in cold water, transfer the parts immediately to a boiling solution conforming to the fol lowing composition: Sodium dichromate (Na2Cr207-2H20) Calcium or magnesium fluoride (CaF2 or MgF2) Water (Note 4) 1.5 lb (180 g) 'h oz (2.5 g) to 1 gal (1.0 litre) Boil the parts in the above solution for 30 min, after which rinse them in cold running water, followed by a rinse in hot water at a temperature of not less than 160"F (71C) nor more than 180F (82C) to facilitate drying. Preferably apply the paint coating immediately after the parts are dry. The solution may be held in a steel tank. N' 5: Causes ofDefective Coatings--The following information is intended to provide guidance on the causes of the most usual defects arising in the application of either Class I, Type I or Class I, Type n coatings: (a) Spotted Coatings are caused by ineffective preliminary degreasing or by the presence ofexcessive surface contamination not removed prior to or during the chrome pickling treatment, or both. (b) Nonadherent Powdery Coatings are caused by: (/) Too long an interval between removal from the chrome pickle and rinsing, (2) Ratio of acid to sodium dichromate too high, (J) Temperature of the solution or of the hot-water rinse too high. (4) Metal improperly degreased, or (5) Solution revivified too many times. 5. Class I, Type IIIs 5.1 Scope--Class I, Type III treatment is applicable to all types and forms of magnesium-base alloys except Ml alloy2 and certain rare-earth alloys similar to EK30A.2 It produces in itself no appreciable dimensional change and is, therefore, applicable to parts machined to fine tolerances. The treat ment is applicable to magnesium containing inserts of, or attached to, other metals, but in such cases the preliminary treatment (5.2) shall be in the bifluoride bath (Solution No. 2) described in 5.2.2. N' 6: Causes ofDefective Coatings--The following information is intended to provide guidance on the causes of the more usual defects arising in the application of coatings from the Class I, Type III treatment. (a) Nonadherent Powdery Coatings are caused by: (1) Over-dilution ofthe hydrofluoric acid or acid fluoride solution, (2) Low pH (less than 4.0) of the dichromate solution, (3) Insufficient precleaning of the metal surface, and (4) Direct contact between the steel tank containing the dichromate solution and the article being treated. (b) Failure to Coat and Nonuniform Coatings are caused by: (1) High pH of the dichromate solution, (2) Low concentration of the dichromate, (i) Insufficient precleaning.of the metal surface, (4) Omission of fluoride treatment, (5) Use of an unsuitable alloy for die treatment, for instance, Ml alloy, (0) Excessive immersion time in the hydrofluoric add solution or use of an H2F2 concentration in the dichromate solution in excess of 0.2%, (7) Insufficient rinsing after the hydrofluoric acid dip, and (8) Insufficient heating of the dichromate solution (minimum temperature shoud be 200F (93C)). 5.2 Procedure--Following cleaning as prescribed in Sec tion 2, treat the parts firsi by immersion at 70 to 90T (21 to 32C) in one or other of the following solutions: 5.2.1 Solution No. I: Hydrofluoric acid (60% H2F2) Water (Note 4) 24 fl oz {187 raJ) to l gal (1 litre) 5.2.2 Solution No. 2: Sodium, potassium, or ammonium acid fluoride (NaHF2, KHF2, or NH4HF2) Water (Note 4) 6% oz (50 g) to i gal (1 litre) Solutions No. 1 and No. 2 may be held in tanks consisting of steel lined with lead or rubber. In solution No. 1, immerse AZ31A and AZ31B alloy parts3 for from 30 s to 1 min; immerse all other alloys for 5 min. In solution No. 2, immerse all the alloys for 5 min. Solution No. 2 is suitable for use with all forms of magnesium alloys except those castings which have not been acid-pickled after blasting; these castings shall be treated in the hydrofluoric acid solution (solution No.- 1). Following one or other of the above treatments, the parts shall be rinsed thoroughly in cold running water and transferred to a solution conforming to the following composition: Sodium dichromate (Na2Cr207-H20) Calcium or magnesium fluoride (CaF2 or MgF2) Water (Note 4) 1 to 1.5 lb (120 to 180 g) 'h oz (2.5 g) to 1 gal (1 litre) 4 Conforming to Class 1, Type II treatments are the AMC "L" process, the Dow No. io process, and Type II treatment of Military Specification MIL-M-3171A. 5 Conforming to Class 1, Type III treatments are the AMC "G" process, the Dow No. 7 process, and the Type III treatment of Military Specification MIL-M-3171A. 223 DUP050297406 # D t732 . Operate the above solution at boiling point and immerse the parts therein for 30 min, following which thoroughly rinse them in cold running water, followed by a hot-water dip to facilitate drying. Preferably, apply the paint coating as soon as possible thereafter. A mild steel tank is suitable for holding the above solution. 5.3 Maintenance ofSolutions: 5.3.1 Fluoride Solutions--Keep the concentration of free hydrofluoric acid in the solutions of 5.2.1 and 5.2.2 constant by the addition, as required, of either hydrofluoric acid or acid fluoride, respectively. See Section 9 for the analytical procedure. 5.3.2 Dichromate Solution--Keep the pH of the dichromate solution within the limits 4.0 to 5.5, or 4.0 to 4.8 in the case of AZ31A or AZ31B alloy,2 by addition of chromium trioxide as required. Maintain the level by the addition of water. Maintain the solution saturated with respect to either magnesium or calcium fluoride by contin uous immersion of a cloth bag containing excess of one or other of these compounds. SURFACE PREPARATION PROCEDURES--ANODIC 6. Class II, Type I (Galvanic Dichromate Treatment)6 6.1 Scope--This treatment produces black coatings of good protective and paint-base qualities, and is applicable to all alloys and forms ofmagnesium, including Ml alloy,2 with or without attachments of other metals. No appreciable dimensional change results, and hence the treatment is also applicable to articles machined to fine tolerances. 6.2 Procedure--Following cleaning as prescribed in Sec tion 2, treat the articles in fluoride solution No. 1 or No. 2 as prescribed in 5.2. Use the latter solution when other metals are attached to the magnesium. After rinsing, immerse the articles in a solution conforming to the following composition: Ammonium sulfate {(NH4)2S04) Sodium dichromate (Na2Cr207 2H20) Ammonia (NH4OH) (sp gr 0.880) Water (Note 4) 4 oz (30 g) 4 oz (30 g) Vi 0 oz (2-d ml) 1 gal (1 litre) Operate the above solution at 120 to 140F (49 to 60C). The articles shall be made the anodes in the solution, with the tank, if of mild steel, acting as cathode, or with separate steel cathodes if the tank is lined with nonmetallic materials. No separate generator is necessary,- but the magnesium parts must be electrically connected with the tank, or with the separate cathode plates through an external connection, taking care that the parts do not make direct contact with the cathode material. 6.2.1 The time of treatment shall be such that a uniform black coating is obtained on the articles. This takes from 10 to 30 min, and the consumption of from 70 to 150 A min/ft2 (929 cm2). An anodic current density of not more than 10 A/ft2 (929 cm2) is desirable. 6.2.2 Following the treatment, rinse the parts thoroughly in cold running water, followed by a hot-water dip to facilitate drying. .6.3 Maintenance ofSolutions: 6.3.1 Fluoride Solutions--Maintain the fluoride solutions as under 5.3.1. See Section 9 for the analytical procedure. 6.3.2 Sulfate-Dichromate Solution--Maintain the pH of this solution between 5.6 and 6.2 by periodic additions of a solution containing 5 weight % of both chromic anhydride (Cr03) and concentrated sulfuric acid (H2S04, sp gr 1.84). 7. Class n. Type II7 7.1 Scope--This treatment is applicable to all forms and alloys of magnesium. Many aluminum alloys will anodically polarize in the treatment solution, and hence magnesium parts with aluminum attachments or inserts can be anodized. With aluminum alloys containing copper, however, the coating of the magnesium will proceed only if the area of the aluminum alloy is small compared to that of the magnesium. Metals other than aluminum or its base alloys shall not be in contact with the magnesium. 7.2 Coating Properties--The anodic coating consists of two phases: the first-formed phase is greenish-tan in color and about 0.0002 in. (5 pm) thick; whereas the second phase, -formed only at higher voltages following the production of the tan coating, is fused and vitreous in nature, dark-green in color, and of thickness about 0.0012 in. (30 pm), causing a dimensional increase of about 0.001 in. (25 pm) per surface. The corrosion-resistance and paint-base characteristics are similar, and excellent for both the above phases. The coating possesses high abrasion resistance, but spalls under compression deformation. The dark-green coating can be partially impregnated with low-viscosity, penetrating, or ganic coating materials, a procedure that considerably re duces its spalling tendency. N' 7--The dark-green coating of Class II, Type II treatments is recommended in preference to the thin tan coating only when: (a) Preliminary removal of surface contamination is not convenient. (b) The highest degree of abrasion-resistance is required from the coating. (c) A dimensional increase (see above) can be tolerated. (d) The article will not be subjected in service to impact, deformation, or flexing likely to cause spalling of the coating. 7.3 Procedure--The thin tan coating is formed with a current consumption and in a time approximately one quarter of that required to form the dark-green coating. The latter forms only after the voltage across the solution has reached the spark potential. During the ensuing coating formation, surface contamination, including graphite, is concurrently removed. Thus, articles intended to receive the dark-green coating need not first be cleaned. On the other hand, the formation of the thinner tan coating does not concurrently remove surface contamination. Since such contamination can seriously reduce corrosion resistance, it is mandatory that a preliminary cleaning, including acid pick ling (2.2) shall be given to articles intended to receive the lower-voltage tan coating. 7.3.1 Rack and clean parts as appropriate (see above), and anodize either by direct or alternating current in an electro lyte conforming to one of the following compositions, respectively: 6 Conforming to Class II, Type I treatment are the AMC "K." process, the Dow No. 9 process, and Type IV treatment of Military Specification MIL-M-3171A. 7 Conforming to Class n. Type II treatment is the Dow No. 17 process. 224 Ammo (NH Sodiun (Na2 Phosph Water The 160T (60C deleft in rui water Prefe: parts 7.4 from to bo type. coatii natin applii varyii 50 A, same altera A-mi IWn resist voltag densit 75 to comp carryi consit time currei 7.4. alloys appre of the can t in. (2 belov vitrec 7.5 use, t on th coatin Al AZ31 AZ61 AZ63 AZ91 AZ92 EK30. ZK60. DU PO 502 97407 ations ure. pH 0f IS of a y'dride 84). is and iically esium dized. r, the of the :sium. t be in (Sts of color Phase, ion of eenin sing a irface. cs are under an be g, or)ly re lents is enient. im the nation, vith a one The 1 has ating e, is e the other as not such l pickve the ;), and iectro.itions. D 1732 Direct Cuirent -.Alternating Current . jynonium acid fluoride (fJH4HF2) -jju dichromate (hia2Cr207 -HjO) phosphoric acid (85% H3P04) ^ater (Note 4) 32 oz (240 g) 13.3 oz (99 g) 11.5 fl oz (90 ml) to 1 gal (1 litre) 40 oz (300 g) 13.3 oz (99 g) 11.5 fl oz (90 ml) to 1 gal (1 litre) rte temperature of the solution shall preferably be from [60F to I80F (71 to 82C). It will not operate below 140F 0'C), but temperatures higher than 180F (82'C) do not Jjgleteriously affect the results. After anodizing rinse the parts jn running cold water, followed by a short immersion in hot water, or by treatment with hot air, to facilitate drying, preferably, apply the paint coating immediately after the parts are dry. 7.4 Power Requirements--A current consumption of from 50 to 500 A-min/ft2 (929 cm2) is necessary, according to both the composition of the alloy being treated and the type of coating desired. Thus, in the case of the dark-green coating on AZ31 alloy, for a 10-min treatment with alter nating current, a current density of 30 A/ft2 (929 cm2) is applied; but greater or lesser currents may be utilized by. varying the time of treatment as, for example, application df 50 A/ft2 (929 cm2) for 6 min. On the other hand, for the same alloy, the thin tan coating may be applied with alternating current, with a current consumption of 75 A-min/ft2 (929 cm2), equivalent to a treatment time of only 1% min at 50 A/ft2 (929 cm2). As the coating forms, the resistance of the circuit increases, and consequently the voltage must be increased to maintain a constant current density. Normally the voltage across the bath will reach from 75 to 95 for the dark-green coating (according to alloy composition) and from 60 to 75 for the thin tan coating. In carrying out the treatment, a constant current control is a considerable advantage, inasmuch as the total treatment time can be preset and manual control of the voltage and current then become unnecessary. 7.4.1 As guides to the current consumptions with various alloys, some data are presented in Table 1. It will be appreciated that rigid current consumptions in the formation of the thin tan coating cannot be specified, since this coating can be varied in thickness considerably between say 0.0001 in. (2.5 pm) and 0.0005 in. (12.7 pm), and still be formed below the critical spark potential at which the dark-green vitreous coating begins to develop. 7.5 Solution Control--With depletion of the bath upon use, the final voltage required to impress the above currents on the article will slowly rise, but even for the full green coating at least 20 ft2 (50 dm2) of surface can be treated per TABLE 1 Current Consumption with Various Alloys Alternating Current Direct Current Alloy Voltage A-min/ft2 (929 cm2) Voltage A-min/ft2 (929 cm2) ark- Thin Dark- Thin Dark- Thin Dark- Thin Green Tan Green Tan Green Tan Green Tan AZ31A or B 90 70 300 75 95. 75 190 50 AZ61A AZ63A 90 6B 400 95 72 300 B0 68 600 ioo 84 72 400 70 AZ91A 75 64 480 80 69 280 AZ92A EK30A 75 90 64 70 600 400 - *" 80 95 69 400 75? - 3ffO ZK6QA 85 70 300 90 75 . 190- gallon (1.0 litre) of solution before any change in the final voltage is experienced; and up to 40 fit2 (98 dm2)/gal (1 litre) can be treated before revivification of the solution becomes necessary. 7.5.1 Prior to revivification, analyze for dichromate and phosphoric acid (see Sections 10 and 12), and make up differences from the original composition by additions of sodium dichromate and phosphoric acid. 7.5.2 A simple method for the determination of fluoride in the solution is not yet available. The fluoride concentra tion, however, is not critical, provided it always exceeds minimum concentration, below which pitting of the articles may ensue during their treatment. When revivifications are made by additions of sodium dichromate and phosphoric acid, make a concurrent addition of ammonium acid fluo ride, equal to three times the weight of sodium dichromate added. Secondly, if pitting of the articles should occur under treatment; it is an indication that the fluoride content of the solution is too low, and about 5 oz (38 g)/gal (1 litre) of ammonium" acid fluoride shall then be added in order to relieve the trouble. 7.6 Tank and Rack Materials--Mild steel is suitable for tanks and heating coils. Other metals, such as copper, aluminum, lead, zinc, Monel, and stainless steels are at tacked by the electrolyte. When direct current is used the tank itself can be the cathode, but, when alternating current is used, at least two magnesium parts are necessary, of area ratios not more than 3 to 1, each one serving as electrode. The articles shall not contact the tank, otherwise pitting will ensue. 7.6.1 Racks shall be normally made of magnesium alloy, but aluminum alloys containing magnesium, such as ASTM alloy No. GR20A, or its Aluminum Association equivalent, alloy No. 5052, can be used if desired, provided they are not allowed to be in the solution on open circuit. Use a spring clip with magnesium ends for providing contact with thin sheet material, the liquid level not being allowed to extend beyond the limit of the magnesium ends of the clip. No solution-line attack is experienced on magnesium. Magne sium racks may be stripped by immersion for 2 min- in hot 20% chromium trioxide solution or by immersion at room temperature for about 8 miri in the chromium trioxidenitrate solution bath described in Section 2.2.3. 8. Class II, Type HI8 8.1 Scope--This treatment is-applicable to all forms and alloys of magnesium, free from attachments or inserts of other metals. 8.2 Coating Properties--The anodic coating consists of two phases; The first-formed subcoating phase is a light tan in color, and causes a dimensional increase of about 0.0002 in. (5 fim) per side; the second and thicker phase, formed at higher voltages, is dark brown and causes a dimensional increase offrom 0.001 in. to 0.0012 in. (25 pm to 30 pm) per surface. The paint-base characteristics are similar, and excel lent for both the above phases. 8.2.1 The dark-brown coating is hard and highly abrasionresistant, but it spalls under compression deformation and its 8 Conforming to Class 11, Type III treatment is the HAE process. 225 DUP050297408 1, D 1732 formation can cause a loss of fatigue strength of the metal. Such loss is negligible with metal erf thickness 0.1 in. (2.5 mm) or over, rising to 3% and 9% for thicknesses of 0.094 in. (2.4 mm) and 0.040 in. (1 mm), respectively, all under reversed bending and corrected for coating thickness. No loss of fatigue strength arises from application of the thin tan coating* and neither is this coating subject to spalling. 8.3 Procedure--Rack and clean with hot alkaline cleaner (2.1) or chromium trioxide (2.2.1), or both, as appropriate, and anodize with alternating current in an electrolyte con forming to the following composition: Potassium hydroxide (KOH) Aluminum hydroxide (AI(OH)3) soluble in hot KOH solution (Note S) Potassium fluoride (K2F2j Trisodium phosphate (Na3P04) Potassium manganate (K3Mn04) (Note 9) Water (Note 4) IS to20 oz(135 to 150 g) 4 oz (30 g) 4.5 oz (34 g) 4.5 oz (34 g) 2.5 oz (19 g) to 1 gal (1 litre) Dissolve the constituents of the electrolyte in the above order. Maintain the temperature of the electrolyte between 77 and 100F (25 to 38C). N' 8--If an exceptionally hard, abrasion-resistant dark-brown coating is desired, the aluminum hydroxide in the above electrolyte shall be increased to 6 to 7 oz (45 to 52 g)/gal (1 litre). N' 9--Potassium manganate (K2Mn04) in the above electrolyte may be replaced with an equal weight of potassium permanganate (KMn04), but in such case the permanganate shall be completely dissolved in water before it is added to the solution and an additional 1 Vi oz (11 g) of potassium hydroxide shall also be added. During operation of the bath, the permanganate is slowly reduced to manganate, complete conversion taking place after a metal area of approximately 2 ft2 (18.6 dm2)/gal (1 litre) of electrolyte has been treated. 8.4 Post-Treatment--After the electrolytic treatment, rinse the parts well in water and immerse for 1 min at room temperature in a solution consisting of 2.7 oz (20 g) of sodium dichromate (Na2Cr207*2H20) and 13.3 oz (99 g) of ammonium bifluoride (NH4HF2)/gaI (1 litre) of solution. Following the immersion, remove the parts and dry without rinsing. Paint at any convenient time after the parts have dried. 8.5 Power Requirements--The practical range from cur rent density is from 15 to 20 A/ft3 (9.3 dm2) with voltages rising to from 70 to 86 (depending on alloy) for the hard brown coating and to 58 V for the thin tan coating. In this current density range, the terminating voltage is reached in from 45 to 60 min for the hard brown coating and in 10 min or less for the thin tan coating. Raise the voltage quickly from zero to 40 or more, and adjust the current and retain at the density desired. Normally the voltage will rise to 55 or more within 1 min, but as the coating forms, the resistance of the circuit increases and the voltage must be raised continu ously to maintain the desired current density; N' 10--If, at low initial voltages, the current remains high and coating formation does not proceed, a "surge" current shall be imposed by rapidly raising the voltage to 40, followed by immediately lowering it to zero. The voltage shall then be adjusted in the normal manner to maintain the desired current density. 8.6 Solution Control--The operating life of the electrolyte is extremely long, and under normal conditions of use it need never be discarded. Manganate and aluminate deplete slowly with use, whereas the depletion of fluoride and phosphate is extremely slow. 8.6.1 In the case ofthe dark-brown coating, a lightening of i the normal color indicates a depletion of manganate in the 1 5solution, and additions shall then be made of 1 oz (7.5 g) of 1 ar potassium manganate plus 1% oz (11 g) of aluminum I jyl hydroxide for each gal (1 litre) of solution. Add the alu- 1 to minum hydroxide after first dissolving it in a solution 1 SO containing a weight of potassium hydroxide equal to that of 1 the aluminum hydroxide to be added 1 in 8.6.2 A rough coating indicates either a low, or an 1 in excessively-high, alkalinity in the electrolyte. The alkalinity [ bt shall be maintained between 10 and 12% free KOH, as * tb determined by the method described in Section 13. I 8.7 Tank and Rack Materials--Plain black iron is suit- | 11 able for tanks and cooling coils. Suspend the parts by | magnesium-base alloy clips or the like and protect them at f lo the solution level by electroplaters' vinyl tape. Magnesium racks may be stripped of coating when necessary by immer T re sion in hot 20% chromium trioxide solution (Note 11). 8.7.1 Divide parts to be treated into two batches each of l: approximately the same surface area. Rack each of the ct batches and connect electrically to one or other of the inlet Pl terminals of the power supply so that the magnesium parts li- constitute both electrodes of the electrolysis bath (Note 12). (I N' 11: Safety Precautions--Consideration should be given to the : health hazards associated with the procedures covered by this specifica tion. Precautions must be taken to avoid skin contact with any of the solutions involved, and to avoid inhalation of vapors, fumes, or spray j arising thereform. Baths containing dichrotnate or fluoride shall be fitted ! with exhausts to remove all spray arising therefrom. j N' 12: Repair Treatments--Pretreatment films that have been ! damaged shall be repaired before painting. Repair shall be effected by ' one of the treatments below. The phosphate touch-up solution of 8.2 - below necessitates special preparation, whereas a chrome pickle solution | is often already available. Nevertheless, for brush-on treatment, the - : phosphate solution possesses the advantages of being nontoxic and nonirritant. ` | (a) Chrome PickleRepair Treatment--The chrome piclde solution for i Class I, Type I treatments (for wrought parts) shall be copiously and ; continuously applied' to the damaged area by brush for at least 1 min. The treated surface shall then be thoroughly flushed with water and, when dry, rubbed vigorously with a clean dry rag to remove loose powdery matter which, if allowed to remain, would deleteriously affect the adhesion of superimposed paint. (b) Phosphate Repair Treatment--A solution shall be used com i forming to the following composition: w A C 1 ft i) h r Monoammonium phosphate (NH4H>P04) Ammonium sulfite ((NHJjSOj-HiO)' Ethyleneglycol monobutyiether . Water (see Note 4) 16oz(84g) 4oz(30g) ' 13to 20floz(101 to 156 ml) 1 gal (1 litre) g> The above solution shall be applied copiously to the damaged area by brush in sufficient quantity to keep the surface wet for at least 1 min, or until a medium to dark-gray continuous coating is formed. The treated metal surface shall then be well flushed with water and allowed to dry j before thepamtis applied: r i t l t ANALYTICAL PROCEDURES 9. Fluoride Solutions 9.1 This method is applicable to the relevant baths of Class I, Type III (Section 5) and Class II, Type I (Section 6) treatments. The concentrations of both hydrofluoric acid (HF) and bifluoride shall be determined by titration with 1N sodium-hydroxide (NaOH) with 1 N sodium hydroxide (NaOH) solution, using phenolphthalein as indicator. 226 DUP050297409 ning of in the 5 g) of ninun, ie alu. jlution that of or an alinity >H, as is suit, rts by lem at tesiunj mmer). ach of of the e inlet i parts e 12). i to the leoifica' of the ir stray )e fitted e been cted by i of 8.2 olution at, the dc and tion for sly and t min. er and, 3 loose y affect con- 56 ml) .rea by nin, or treated to dry ths of ion 6) ; add iliV oxide \ D1732 ' 9.2 Maintain the hydrofluoric add solution described in , j by additions of fresh acid to give a titration ofbetween 10 20 ml of 1 N NaOH solution per 2 ml of sample. Maintain the bifluoride solution described in 5.2 so that 10 jjl thereof gives a titration of 4.5 to 5.5 ml of 1 N NaOH solution. 9.3 For the hydrofluoric add the sample shall be drawn to a wax-lined pipet, discharged therefrom into at least 100 Ll of distilled water, and titrated immediately. A rubber bulb, or a length of rubber tubing fitted to the suction end of jj,e pipet, shall be used in drawing the sample into the pipet. jO. Dichromate Solutions 10.1 This method is applicable to solutions of the fol lowing treatments: Class I, Types I, II, and III; and Class II, Xypes I and II (Sections 3, 4, and 5; and Sections 6 and 7, excess of sodium hydroxide, such excess being titrated with standard acid. Interference from fluoride is prevented by converting it to fluoborate, by addition of boric acid. 12.2 Molybdate Reagent--Prepare as follows: mix 118 g of 85% molybdic acid (H2Mo04) with 400 ml of distilled water, add 80 ml of ammonium hydroxide (NH4OH) solution (sp gr 0.880) with stirring, and filter when solution is complete. Slowly pour the filtrate, with stirring, into a cold mixture of 400 ml of concentrated nitric acid (HN03, sp gr 1.42) and 600 ml of water. Allow the solution to stand over night, and filter. 12.3 Procedure--Dilute a 14-ml weighed sample of the solution under examination to 500 ml, and then further dilute 50 ml of this diluted solution to 500 ml. Then again dilute 25 ml of the latter solution to 100 ml, and add 10 g of ammonium nitrate (NI^NO^, 1 g of boric acid (H3B03), respectively). 10.2 Add 1 ml of the dichromate solution concerned to [50 ml of distilled water, and mix therewith 5 ml of concentrated hydrochloric acid. (HC1, sp gr 1.19) and 5 g of potassium iodide (KI). After at least 2 min, titrate the liberated iodine in the solution with 0.1 N sodium thiosulfate--(Ma2S203) solution using starch as an internal indicator. 10.3 Calculation: and 15 ml of concentrated nitric arid (HN03, sp gr 1.42). Heat the mixture to 104F (40C) and slowly add 40 ml of molybdate reagent. Allow the resulting precipitate of ammo nium phosphomolybdate to stand for 30 min, and then filter through a fine-texture, low-ash paper. Wash the precipitate free from acid by means of a 1% solution of potassium nitrate (KN03), and mix, together with the filter paper, with an excess of 0.1 N sodium hydroxide (NaOH) solution, using A x 0.0415 = B A x 4.96 = C where: A - millilitres of 0.1 N Na2S203 solution, g = pounds per gallon of sodium (Na2Cr207 2H20), and C - grams per litre of sodium dichromate. dichromate phenolphthalein as indicator. Titrate the excess of NaOH with 0.1 N hydrochloric acid (HC1). 12.4 Calculation: Phosphoric acid (H3P04), % = [(A- B)/C] x 0.426 where: A = millilitres of 0.1 N NaOH solution, B = millilitres of 0.1 N HQ, and C = grams of sample in aliquot. 11. Nitric Acid Solution 11.1 This method is applicable to Class I, Types I and II treatment solutions. 11.2 Mix 50 ml ofdistilled water with 1 ml of the solution in question, and titrate the mixture with 0.1 N sodium hydroxide (NaOH) solution to a pH of 4.0 to 4.05, using a pH meter with a glass electrode. 11.3 Calculation: Ax 0.0505 = B A x 6.34 = C 13. Free Alkali 13.1 This method is applicable to the Glass II, Type III solution. Manganate, fluoride, and phosphate are precipi tated by barium nitrate addition, and the filtrate therefrom is titrated with standard arid. 13.2 Pipet a 2-ml sample of the solution under examina tion into a 25-ml glass-stoppered graduated cylinder, fol lowed by addition of 10 ml of 0.25 N sodium hydroxide (NaOH) solution and 0.5 g of barium nitrate (Ba(N03)2) crystals. Shake this mixture vigorously for 1 min, filter where: A = millilitres of 0.1 iVNaOH solution, and B = pints per gallon of nitric acid (HN03), C = millilitres of 70% nitric acid per litre. through a medium-texture, low-ash paper, and wash the precipitate free from alkali, preserving all filtrate. Using a pH meter with a glass electrode, titrate the free alkali in this filtrate to pH 10.5, with 0.25 N hydrochloric arid (HQ). 12. Phosphoric Acid Solution 12.1 This method is applicable to the Class II, Type II treatment solution. The phosphoric acid is precipitated as ammonium phosphomolybdate, which is dissolved in an 13.3 Calculation: Potassium hydroxide, % -- 2.805 x [(A/4) -- 2.5] where: A = millilitres of acid used. The American Society for Testing and Materials takas no position respecting the validity of any patent rights asserted in connection with any Item mentioned In Otis standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either forrevision of this standardor for additional standards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical committee, which you may attend # you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103, 227 DUP050297410 I (jOlM Designation: D 1734 - 63 (Reapproved 1980)e1 Standard Method of Making and Preparing Concrete and Masonry Panels for Testing Paint Finishes1 This standard is issued under the fixed designation D 1734; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This method has been approvedfor use by agencies ofthe Department ofDefense andfor listing in the DoD Index ofSpecifications and Standards. el N' --Editorial changes were made in Sections 2.1 and 5.3 on October 1980. 1. Scope 1.1 This method describes the procedures and materials required in making concrete and masonry panels for use in testing paint finishes designed for either Portland cement concrete or stucco surfaces. 2. Apparatus 2.1 White Asbestos Cement Shingles, 12 by 24 in. {305 by 610 mm) in size, or asbestos cement sheet, lh in. (3.12 mm) thick, of the required size. 2.2 Forms, wooden or rustproof metal, to make panels of the required size. 2.3 Container, of wood, stainless steel, or other rustproof metal of sufficient size to mix the mortars. 2.4 Notched or Serrated Applicator, similar to those used in applying cement for tile or linoleum flooring. 2.5 Miscellaneous Equipment--Wooden or cork trowel, wooden screed, steel trowel and 3-in. (76-mm) wide stiffbristle paint brush. N' 1--Wooden trowels, screeds or containers may be made of seasoned oak which may be rendered nonabsorptive by immersion for 15 min in paraffin at 220 C (392 F) in accordance with ASTM Method C 227, Test for Potential Alkali Reactivity ofCement-Aggregate Combi nations (Mortar Bar Method).2 3. Materials 3.1 Portland Cement, conforming to the requirements of Type I of ASTM Specification C 150, for Portland Cement,2 3.2 Masonry Cement, conforming to the requirements of Type II of ASTM Specification C 91, for Masonry Cement2 3.3 Natural Sand, conforming to the requirements of ASTM Specification C 144, for Aggregate for Masonry Mortar,3 modified as follows: 3.3.1 The standard sand may provide too coarse a texture on portland cement concrete panels. If smoother texture is desired, the requirement of the specification that not more than 35 % shall pass the No. 50 (300-ji.m) sieve should be waived, and the sand should be required to contain from 50 : J This method is under the jurisdiction of ASTM Committee D- L on Paint and Related Coatings and Materials. Current edition accepted Sept 30, 1963. Originally issued 1960. Replaces D 1734-60 T. 2 Annual Book ofASTM Standards, Vols 04.0! and 04.02. 3 Annual Book ofASTM Standards, Vols 04.02 and 04.05. to 60 % passing the No. 50 sieve, and from 5 to 20 % passing the No. 100 (150-pm) sieve, with the other provisions of grading remaining unchanged. 3.3.2 The standard sand will provide aggregate too large for a,_satisfactory masonry cement (stucco) mortar mixture. Satisfactory sand may be obtained by requiring that 100 % pass the No. 16 (1.18-mtn) sieve, from 45 to 80 % pass the No. 30 (600-pm) sieve, from 65 to 75 % pass the No. 50 sieve, and from 10 to 30 % pass the No. 100 sieve. 3.4 Water, of sufficient purity as to be potable. 3.5 Resin Emulsion* 4. Size of Test Panels 4.1 For use on outdoor testing racks, the panels shall be 8 by 12 by 3/g in. (203 by 305 by 9.5 mm) in size. 4.2 For machine exposure tests, the panels shall be of a size to fit the apparatus to be used for such tests. The panels shall be Vs in. (9.5 mm) in thickness and should have a surface area of not less than 18 in.2 (116 cm2). 5. Application of Bond Coat 5.1 Prepare forms of correct size for panels to be made and place upori a wooden platen or table. The forms should be oiled or waxed before use. 5.2 For ease in removing the finished test panel, make the forms easily demountable, or equip the table upon which panels are made with several plungers, operated by foot pressure, which may be used to force the completed panel up and out of forms easily. 5.3 Cut the asbestos-cement shingles or the asbestoscement sheet in rectangles V32 in. (0.8 mm) under the required panel size to provide a slip fit within the forms. (Caution--Use vacuum dust collector for removal of asbes tos-cement particles during cutting,) 5.4 For each square foot of panel to be made, make up a hond coat consisting of 60 g of sand, 20 g of cement, 8 gof water, and 20 g of emulsion. 5.5 In the mixing box, thoroughly mix the sand and cement (dry), then add the water. After thoroughly mixing, add the emulsion and mix until homogeneous. = j 4 Emulsion Rhoplex AC-33 obtainable from Rohm & Haas Co., Independence Mall W,, Phila., Fa., or Resyn 12K51 obtainable from the National Starch cr.d Chemical Corp., 1700 W. Front St, Plainfield, N. J,, or equivalent resin emulsion are satisfactory for this purpose. 5.6 Wet surface of t about 5 mi 5.7 Disti previously either a br notches apj 5.8 Cleat coating, so apply the c< 5.9 Alio' imum). 6. Preparai 6.1 In tb of Portland oughly mi: thoroughly, sufficiently the form. N' 2--> mix may be < weight ofwat< 6.2 Place side up, wit on top of i mixture int top with a t trowel to le' Finally, bru N' 3--1 may be wette water-cement and sloppy m DUP050297411 % passing risions of too large mixture, at 100 % pass the 2 No. 50 hall be 8 be of a e panels have a e made should ike the which Y foot riel up >estosjr the forms, asbes- e up a 8 g of d and lixing, D 1734 36 Wet the smooth or back side of-the shingle, or the ^ace of the sheet to which the bond coat will be applied, 5j,oUt 5 min before applying the bond coat. 3 5.7 Distribute the required amount ofbond coat upon the j^iously wetted shingle or asbestos cement sheet, using ,tber a brush, or a notched applicator or scraper, having notches approximately '/s in. (3.2 mm) deep. 5.8 Gean the edges of the panel immediately after gating, so that the panel will fit in forms when ready to aPP^the concrete or "asonry mix. 5.9 Allow the bond-coated panel to stand overnight (min imum). 6. preparation of Concrete Panels 6.1 In the mixing box, prepare the concrete, from 1 part 0f portland cement and 3 parts of sand by volume. Thor oughly mix these dry ingredients. Add water and mix thoroughly. Use only enough water to make the mortar sufficiently plastic as to be easily worked into the comers of the form. jjC N' 2--Using dry ingredients, a good portland cement concrete mix may be obtained by using sufficient water to give a ratio between weight ofwater and weight ofcement ofapproximately 0.6 (0.1) to 1.0. 6.2 Place the previously coated shingle or sheet, coatedside up, within the forms. Place the wet concrete in the forms on top of the coated base with the steel trowel, work the mixture into the comers and next to the form. Strike off the top with a wooden screed and use a wooden or cork float or trowel to level offthe surface and work to the desired texture. Finally, brush the surface evenly with the dry paint brush. N' 3--IF deemed desirable, the surface of the bond-coated base may be wetted prior to placing the concrete mix. If this is done, the water-cement ratio should be reduced to compensate, otherwise a wet and sloppy mix may result. 6.3 During the first hour of the setting period, gas may form between the bond coat and the concrete coat, causing bubbles to form upon the surface of the panel. These should be broken carefully or punctured by a slender, sharp instru ment to permit the gas to escape. Any holes thus made may be smoothed over, or filled up, about an hour later. 6.4 After the concrete has set up sufficiently to permit removal of the forms from the panel, or the panel from the forms, smooth the edges to desired texture, and cover with a wet cloth. 6.5 Keep the panel covered with the wet doth until seasoned to desired age, wetting the cloth thoroughly twice daily. To provide freedom from crazing or cracking, a minimum seasoning period of seven days is recommended. 6.6 Before using, bevel off top exposed edges with a carborundum stone, sufficiently to prevent edge-breakage in use. ' 7. Preparation of Masonry Panels 7.1 In~the mixing box, prepare the masonary or stucco mix from 1 part of Portland cement, 1 lA parts of masonry cement, and 3 parts of sand, by volume. Thoroughly mix these dry ingredients. Add water and mix thoroughly. Use only enough water to make the mortar suffitiently plastic as to be easily worked into the comers of the form. N' 4--The addition ofmasonry cement to the stucco mix makes a more workable mix than using only portland cement, and the watercement ratio may be reduced to 0.5 (0.1) to 1.0. 7.2 Proceed as described in Section 6.2 to 6.6. 8. Identification 8.1 Identify the back of each panel (shingle or asbestos cement sheet side) as to type of mix (concrete or masonry) and data of manufacture. N' 5--For optimum reproducibility, panels used in the same test should be of the same age, cure and seasoning. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk oi infringement ofSuch rights, are entirely their own responaibtlity. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your commentsare Invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technbal committee, which you may attend. U you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St, Philadelphia, PA 19103. indence rch and nulsion 229 DUP050297412 i Designation: D 1735 - 87 should be agi Standard Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus1 N' 2--Aj substrates arc Methods D82 uniform films. 7. Procedure This standard is issued under the fixed designation O 1735; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 7.1 Fill tfc Type III of S 7.2 Maint 1. Scope 1.1 This practice covers the basic principles and operating procedures for testing water resistance of coatings in an apparatus similar to that used for salt spray testing. 1.2 This practice is limited to the methods of obtaining, measuring, and controlling the conditions and procedures of water fog tests. It does not specify specimen preparation, specific test conditions, or evaluation of results. N' I--Alternative practices for testing the water resistance of coatings include Practices D 870, D 2247, and D 4585. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and D3359 Test Method for Measuring Adhesion by Tape Test3 D3363 Test Method for Film Hardness by Pencil Test3 D4585 Practice for Testing Water Resistance of Coatings Using Controlled Condensation3 3. Summary of Practice 3.1 Coated specimens are placed in an enclosed chamber where a water fog is sprayed on them. The temperature ofthe chamber is usually maintained at 100F (38C). The expo sure condition is varied by selecting the duration of the test. Water permeates the coating at rates that are dependent upon the characteristics of the coating. Any effects such as color change, blisters, loss of adhesion, softening, or embrittlement are observed and reported. 2F (38 : temperature 7.3 Suppc from the ver the direction for flat spec specimens, f other, any acting as a \ one specime 7.4 Place fog for met nozzle with place them .* Glass funne ders or disl establish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. 2. Referenced Documents 4. Significance and Use mended. 4.1 Water can cause the degradation of coatings, so knowledge of how a coating resists water is helpful in predicting its service life. Failure in water fog tests may be I 7.5 Adju; of water/h i mm. 2.1 ASTM Standards: B 117 Method of Salt Spray (Fog) Testing12 D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products3 D 610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces3 D714 Test Method for Evaluating Degree of Blistering of Paints3 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 . D 870 Practice for Testing Water Resistance of Coatings Using Water Immersion3 D1193 Specification for Reagent Water4 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting5 D2247 Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity3 D2616 Test Method for Evaluation of Visual Color Difference With a Gray Scale6 caused by a number of factors including a deficiency in the N' 3--1 coating itself, contamination of the substrate, or inadequate i mL/h for a cc surface preparation. The test is therefore useful for evalu ating coatings alone or complete coating systems. 7.6 Oper 4.2 Water fog tests are used for research and development closed unit of coatings and substrate treatments, specification accep tance, and quality control in manufacturing. These teste usually result in a pass or fail determination but the degree of failure may also be measured. A coating system is considered ; to pass if there is no evidence of water-related Mure after a specified period of time. 4.3 Results obtained from the use of water fog tests in accordance with this practice should not be represented as being equivalent to a period of exposure to water in the natural environment, until the degree of quantitative corre lation has been established for the coating or coating system. 4.4 The test apparatus is identical to that used in Method B 117, and the conversion of the apparatus to water fog testing is not difficult. Corrosion tests of a scribed coating on a ferrous substrate are possible as the water that drips off of | the specimens is not recirculated. ! 1 This practice is under the jurisdiction ofASTM Committee O-1 on Faint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.27 on Accelerated Testing. Current edition approved Nov. 27, 1987. Published January 1988. Originally published as D 1735 - 60 T. Last previous edition D 1735 - 86a. 1 Annual Book ofASTM Standards, Vols 03.02 and 06.01. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vols 02.05 and 06.01. 6 Annual Book ofASTM Standards, Vol 14.02. 5. Apparatus 5.1 Test Chamber, Test Specimen Supports, and Fog Collecting Devices, as specified in Method B 117. 6. Test Specimens 6.1 This practice does not cover the preparation of test specimens. The substrate composition and surface prepara tion, specimen preparation, and the number of specimens 230 DUP05029741 3 by Tape il Test3 Coatings chamber ure of the 'he expof the test, ependent s such as ning, or tings, so alpful in ; may be cy in the adequate :r evalu- lopment n accepese tests degree of nsidered after a :ests in ited as in the corresystem. Method ater fog ating on ps off of D 1735 sj,ould be agreed upon prior to testing. - N' 2--Applicable methods for the preparation of test panels and s#t)Strates are given in Methods D 609 and Practices D 1730. Test Methods D 823 cover application techniques of the production of [inform films. j. Procedure 7.1 Fill the reservoir with reagent water conforming to fype III of Specification D 1193. 7.2 Maintain the test chamber at a temperature of 100 2"F (38 1C). Other temperatures may be used if the temperature is reported in Section 8. 7.3 Support or suspend specimens approximately 15 from the vertical with the plane of the specimen parallel to tfre direction of fog flow. Slotted wood supports are suitable for flat specimens. Provide for free settling of fog on all specimens. Space specimens so that they do not touch each other, any metallic material, or any material capable of acting as a wick. Arrange the specimens so that water from one specimen does not drip on other specimens. 7.4 Place two containers within the chamber to collective fog for measurement. Locate one container near the fog nozzle with the other as far as possible from the nozzle and place them so that they collect only the fog from the nozzle. Glass funnels with the stem extending into graduated cylin ders or dishes having a diameter of 100 mm are recom mended. 7.5 Adjust the atomizing air supply so that 1.5 to 3.0 mL of water/h is collected , in a collector with a diameter of 100 mm. N' 3--The fog rate specified in Method B 117 is only 1.0 to 2.0 mL/h for a collector with a diameter of 100 mm. inspect or remove specimens or to replenish the water supply are permitted. 7.7 Conclude the test after a specified period of time or after effects from exposure to water fog are observed. > 7.8 Wipe the test specimens dry. Rate specimens for changes in color, blistering, etc. Evaluate specimens no less than 5 min and no more than 10 min after removal from test, as the effects from water exposure can change within a short time. Remove only as many specimens as can be rated within the specified time. N' 4--The 0 to 10 scale described in the ASTM STP 5007 is preferred for rating. Relevant procedures for evaluating water effects are described in Test Methods D 610, D 714, D 2616, D 3359, and D 3363. 7.8.1 If possible, rate the specimens again after they have been removed from the test for a recovery period long enough that moisture absorbed within the specimens dries out and the specimens reach moisture equilibrium with room air. A recovery period of 12 from 24 h is generally sufficient.- The post-recovery rating allows evaluation of the permanent effects of the exposure as distinct from the transient effects, and is especially important for evaluation of color and gloss. 8. Report 8.1 Report the following information: 8.1.1 Sample identification. 8.1.2 Results of the evaluation(s). 8.1.3 Reference to Practice D 1735. 8.1.4 Hours of test duration. 8.1.5 Test temperature. 8.1.6 Rate of fog collection and pH of water collected. 8.1.7 Special conditions of test or any deviations in test procedure. 7.6 Operate the test continuously with the test chamber closed unless otherwise specified. Short interruptions to 7Paint Testing Manual, ASTM STP 500, ASTM, J 972. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity at any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at.any time by the responsible technical committee and must be reviewed every five yeans and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments witl receive careful consideration at a meeting of the responsible technical committee, which you may attend. It youJeel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. nd Fog i of test preparaecimens 231 DUP0502 97414 i Designation: D1736 - 89 Standard Test Method for nonuniform i: panels. If the ered unaccept Efflorescence of Interior Wall Paints1 JO. Procedure This standard is issued under the fixed designation D [ 736; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the tendency of an interior wall paint to effloresce under normal environmental conditions. Historically this phenomenon has been exhibited primarily with latex, or other water-based paints, and the method has been used in testing aqueous products. 1.2 This test method is limited to the determination of the efflorescence resulting from migration of soluble salts from within the paint film. It does not deal with the efflorescence attributable to certain substrates. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D 1193 Specification for Reagent Water12, 3. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 efflorescence--a condition that occurs when soluble salts in the dried paint film or in the substrate migrate to the film surface during exposure. It should not be confused with other causes of nonuniform appearance or whitening that may occur at the time of application. Efflorescence is seen as either a light, medium, or heavy deposits of crystals. It exists both in isolated patches and over wide areas. Another evidence of efflorescence is the development of a nonuniform appearance of flat or glossy areas during the cycling procedure of the test. 3.1.2 degrees ofefflorescence: 3.1.2.1 flatting and glossing--A nonuniform decrease or increase in gloss noticeable when the surface is illuminated and viewed at near grazing angles. There is no apparent change in color when viewed perpendicularly to the surface. 3.1.2.2 fine efflorescence--A barely discernible whitening of the surface when viewed perpendicularly. 3.1.2.3 medium efflorescence--A readily noticeable whit ening of the surface without a marked masking of the color. 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.42 on Architectural Finishes. Current edition approved March 31, 1989. Published May 1989. Originally published as D1736-60 T. Last previous edition D 1736 - 89(1984)**. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3.1.2.4 heavy efflorescence--A white deposit sufficient to mask the color. - 4. Summary of Test Method 4.1 Painted panels are exposed to controlled cycles of low temperature and high humidity, and to standard conditions of temperature and humidity, inducing a fine condensate on the surface. The test is run for a maximum of eight cycles. f 5. Significance and Use' 5.1 TJie test conditions are similar to conditions that produce efflorescence inside a home or building. The degree of efflorescence and the number of cycles required to produce it are a good indication of the paint's ability to resist efflorescence. 6. Apparatus 6.1 Test Cabinet--A cold-wall type of household refriger ator without exposed cooling coils. Additional humidity shall be introduced into the test area from a pan of water on the chamber floor, or by putting water in the butter conditioner and setting die conditioner at its highest temperature. Conditions in the test cabinet shall be maintained at 42 3F (5.5 1.5Q and at 75 to 80 % relative humidity. Any other type of cabinet, used should be checked for reproduc ibility of. test results by comparison with a recommended cabinet. i 7. Reagents 7.1 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type IV of Specification D 1193. 8. Test Panels <> 8.1 A sealed substrate shall be used. One satisfactory surface is tempered hardboard sealed with one coat of shellac varnish (3 to 4-lb cut). The panel size shall be 6 by 18 in. (150 by 450 mm). If the panel does not fit the cabinet, the size may be changed, although the area should be kept approximately the same. 9. Preparation of Panels 9.1 Apply the shellac varnish to the test panel and allow to dry. Brush two coats of the test paint on both sides of the sealed panel. Apply the test paint at a temperature above 60F (15.5Q and allow approximately 1 h between coats or, if not a latex paint, allow an appropriate time for drying between coats. After applying the second coat, dry the panel for 1 h (or appropriate time) at the same temperature and observe for uniformity of appearance at all angles of viewing before placing in the test cabinet If the panels are 10.1 Hang spacing of 1 t for 23 h. Thei (25'C) and 5( (approximate! 10.2 Inspec an 85' angle c in surface apt 10.3 Retur 80 % relative steam treatmi 10.3.1 Hea flat-bottom p there is no bi 10.3.2 Rer over the pan soon as the f area return t should take < and the pane than 5 to 10 N' 1--Pt cabinet. The pa with the format test cabinet too 232 DUP050297415 ient to Of low Jitions ate on ycles. s that degree 'ed to > resist frigery shall on the tioner 'ature. 42 Any oducended referter as # D 1736 [ -uniform in gloss or color, reject them and prepare new ! 8 oeis. if the condition persists, the paint should be consid- ^ unacceptable for testing. (P procedure jO.l Hang the panels vertically in the test cabinet with a cing of 1 to 2 in. (25 to 50 mm) between them and chill 23 h. Then place them in a room at approximately 77F LoC) and 50 % relative humidity until the surface is dry approximately 30 min). ' 10.2 Inspect for efflorescence by observing the panels at 85* angle of incidence to a light source so that any change . surface appearance can readily be noted. 1 10.3 Return the panels to the test cabinet at 42F (5.5"C), UP % relative humidity for '/> h to chill before receiving a jteam treatment as follows: 10.3.1 Heat Vi in. (13 mm) deep reagent water in a Oat-bottom pan to boiling. Remove or reduce the heat until (Here is no bubbling. 10.3.2 Remove the panel from the cabinet and hold it over the pan until afine condensate forms on the surface. As" soon as the fine condensate covers about 75 % of the panel area return the panel immediately to the test cabinet. It should take only a few seconds to develop the condensate, and the panel should be replaced in the test cabinet in less than 5 to 10 s. N' 1--Place the steam apparatus as near as possible to the test cabinet. The panel temperature will rise quite rapidly and will interfere ^jlh the formation and retention of condensate if the panel is out of the test cabinet too long. Formation of too large a condensate droplet will cause water spots or rundown streaks and interfere with the develop ment and rating of efflorescence. 10.4 Subject the panels to eight cycles, unless heavy efflorescence is observed in fewer cycles. The 23 h in the test cabinet followed by conditioning at standard temperature and humidity and by observation of the panels constitute the first cycle; the steaming, 23-h chilling, conditioning, and observation constitute subsequent cycles, with exposure in the test cabinet over the weekend constituting one test cycle. Start the test on Monday or Tuesday so that only one weekend cycle is included in the test series. Other end points may be established by agreement between the purchaser and the manufacturer. 11. Report 11.1 Report any glossing, flatting, light, medium, or heavy efflorescence, and the percent of the surface covered. When heavy efflorescence occurs in fewer than eight cycles, report the number of cycles required to produce this condition. 12. Precision 12.1 This test method was developed to provide a reliable qualitative and semiquantitative measure of efflorescence. Available information on the method is not sufficient to establish its reproducibility on a quantitative basis, so that a statistical statement of precision is not possible. However, the need for other than a reliable qualitative or semi quantitative rating is not apparent at this time; further studies will be undertaken if the need arises. 13. Keywords 13.1 efflorescence The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users o1 this standard are expressly advised that determination of the validity oI any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ;tory icllac 18 in. it, the : kept low to of the above ats or, irying panel e and ewing DUP050297416 Last ASTM Designation: D 1737 - 85 Standard Test Method for Elongation of Attached Organic Coatings With Cylindrical Mandrel Apparatus This test method covers the determination by the cylindrical test apparatus of the elongation of attached organic coatings when applied to flat sheet metal of uniform surface texture. Formerly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials. This test method was discontinued in 1988 and replaced by ASTM Test Methods D 522, for Mandrel Bend Test of Attached Organic Coatings.1 1 Annual Book ofASTM Standards, Vol 06.01. j. S( 1.1 ' that nu descrip such pt N' failures methods linseed-c i 2. Typ I 2.1 l films a 'This and Rela mittee P< Curre: publishec 234 DU P 050297417 Designation: D 1848 - 88 Standard Classification for Reporting Paint Film Failures Characteristic of Exterior Latex Paints1 This standard is issued under the fixed designation D 1848; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. I Scope 1.1 This classification covers descriptions of properties that may be observed in weathered latex paint films. These descriptions should be used in reporting the condition of such paint films. N' 1--In inspecting weathered exterior latex paints, defects or fuflures in the films may be observed that are not described in ASTM methods for evaluating the deterioration of exterior paints of the linseed-oil type. 2. Types of Defects 2.1 The following types of defects of exposed latex paint glnis are recognized: This classification is under thejurisdiction ofASTM Committee D-l on Paint uat Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.42 on Architectural Finishes. Current edition approved Oct. 31,1988. Published December 1988. Originally published as D 1848 - 61 T. Last previous edition D1848 - 63 (1984)el. 2.1.1 Efflorescence, characterized by a commonly white, nonuniform powdery incrustation not readily removed by wiping. Usually it cannot be removed with water only but can be removed with dilute mineral add. 2.1.2 Mottling {or Blotching)--The presence of irregularly shaped and randomly distributed areas of nonuniform ap pearance in color, gloss, or sheen. 2.1.3 Water Spotting--Nonuniformities in color, gloss, or sheen in the shape of spots or streaks, caused by drops or rivulets of water. 2.1.4 Crawling--Defect in which the wet film recedes from small areas of the substrate (usually caused by insuffi cient wetting) leaving those areas uncoated. 2.1.5 Pinholing--The presence of a series of fine holes or voids in the film. 2.1.6 Mud-Cracking, characterized by an irregular broken network of cracks in the film. 3. Index Terms . 3.1 This standard is indexed under the following terms: exterior paints/coatings; latex paints. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, eitherreapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., PhlladelpNa, PA 19103. 235 DUP05029741 8 dOlM Designation: D 1849 - 80 (Reapproved 1987)n Standard Test Method for Package Stability of Paint1 This standard is issued under the fixed designation D 1349; the number immediately following the designation indicates the year of original adaption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 3018 ofFederal Test Method Standard No. 141A andfor listing in the DoD Index ofSpecifications and Standards. flNoTE--Editorial changes were made throughout in May 1987. 5.2.4 ( designate 10 = 8= 6- 6. Precis 6.1 Ed ings by c 1. Scope 1.1 This test method covers the change in consistency and certain other properties that may take place when packaged paint of either the solvent-reducible or water-reducible type N' 1--Containers should preferably be no larger than 1 qt (1 L). N' 2--Storage for 1 month at 125 2F (52 l'C) simulates some ofthe effects of storage for 6 months to 1 year at 73 3.5T (23 + 2C). However, h should be recognized that storage at 125F may not simply accelerate changes occurring at -73"F; with latex paints, foT i is stored at a temperature above freezing. example, at 125"F the growth of some putrefying bacteria is inhibited. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. ' 4.2 Bring the stored sample to 73 3.5F (23 2T), Note evidence of pressure or vacuum in the unopened container. Open the container and note skinning, corrosion and odor of putrefaction, rancidity or souring. Disregard other odors. If the sample is in a 1-qt (1-L) or smaller container, measure the character of the lower or settled layer i f 2. Referenced Documents with the spatula as described in Method D 869. If the sample ' 2.1 ASTM Standards: D562 Test Method for Consistency of Paints Using the Stormer Viscometer2 D 869 Test Method for Evaluating Degree of Settling of Paint2 is larger than 1 qt, omit this step. Hand stir the paint 300 stirs in 2 min with a spatula appropriate to the container, stirring so as to ensure uniform distribution of any settled material (Note 3). Immediately after stirring, measure the consistency of the paint as prescribed in Test Method D 562: without allowing the paint to reset after stirring. j 3. Apparatus 3.1 Spatula, weighing 45 1 g with square-ended blade 43A in. (120 mm) in length and approximately 13/is in. (20 mm) in width as described in Method D 869. 3.2 Viscometer--A Stormer viscometer with the paddle- 4.3 Apply the stored paint to one test panel and the control paint to the other. After the brushed film has completely dried, examine it for grains V32 in. (0.8 mm) in diameter, even larger gelatinous lumps, and streaks caused by such grains or lumps. j ' j type rotor as described in Test Method D 562. 3.3 Paint Brush, 1-in. (25-mm) nylon. . 3.4 Test Surface--A smooth-surfaced paper chart coated N' 3--Avoid the use of a mechanical shaker or syringe-type measuring device that may disperse these lumps. with a suitable varnish or lacquer so as to render the surface impervious and resistant to paint liquids. 5. Report 4. Procedure 4.1 Obtain duplicate samples of the paint in original, unopened containers (Note 1). Examine one of the samples received for the characteristics listed in 4.2, using the procedures therein described. Weigh the other unopened sample to the nearest 1 g, then hold it undisturbed for specified periods of time and ranges of temperature, as agreed between purchaser and seller (Note 2). After storage, reweigh the sample without shaking to determine loss of weight resulting from faulty closure. 5.1 For the stored sample only, report the time of storage I in days and the temperature of storage in degrees Fahrenheit or Celsius. Report the initial and final sample weight. 5.2 For both the sample tested as received and the stored f sample, report the following: ? 5.2.1 Skinning, pressure, corrosion of the container, and ! odor of spoilage, each quality separately designated as \ follows: 10 = none 8 = very slight 6 -- slight 4 ss moderate \ ? 2 = considerable 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom 0 - complete failure 5.2.2 Rigidity of the lower layer as determined in accord- mittee DO1.42 on Architecture] Finishes. Current edition approved Aug. I, 1980. Published September 1980. Originally published as D 1849 - 61 T, Last previous edition D 1849 - 79. 2 Annual Book ofASTM Standards, Vol 06.01. ance with Method D 869, if performed; | 5.2.3 Consistency as the weight in grams necessary t01 produce 200 r/pm on the Stormer viscometer; e 236 1L DUPO 50297419 Ut(l L). ) simulates 1.5"F (23 F may not paints, for inhibited. i 2C). unopened corrosion Disregard r smaller tied layer le sample : 300 stirs r, stirring material nsistency : without and the film has > mm) in cs caused vringe-type D 1849 5.2.4 Grains, lumps, or streaks in the brushed film, designated as follows: 10 = none 8 = very slight 6 = slight 4 = moderate 2 = considerable 0 = complete failure : Precision 1 Empirical Ratings--Reproducibility of empirical ratby different operators cannot be predicted with reli ability because of the personal factor as, for example, in the judgement of odor. 6.2 Lower Layer Rigidity, 4 grades, within one-labora tory. 6.3 Stormer Consistency, 60 g, within one laboratory. 7. Index Terms 7.1 This test method is indexed under the following terms: package stability; stability--package. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination at the validity of any such patent tights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and It not revised, eitherreapproved or withdrawn. Your comments are Invited either tor revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ' storage irenheit it. he stored iner, and nated as n accordessary to 237 DUPO 502 97420 r Designation: D 1978 - 91 I Standard Guide for Analysis of Electrocoat Bath Samples1 This standard is issued under the fixed designation D 1978; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This guide covers the selection of test methods for determination of the important parameters that affect the performance of electrocoating paints. 1.2 The test methods involved are D4370, D4399, D4584, and D 5145. 2. Referenced Documents 2.1 ASTM Standards: D 4370 Test Methods for Acid and Base Milliequivalent Content of Electrocoat Baths2 D4399 Test Method for Measuring Electrical Conduc tivity of Electrocoat Baths2 D4584 Test Method for Measuring Apparent pH of Electrocoat Baths2 D 5145 Test Method for Nonvolatile and Pigment Content of Electrocoat Baths2 3. Significance and Use 3.1 This guide indicates test procedures recommended for the maintenance of acceptable performance of the paint in an electrocoating bath. Several critical parameters must be 1 This guide is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DOl .21 on Chemical Analysis of Paints and Materials. Current edition approved Feb. 22, 1991. Published April 1991. 2 Annual Book ofASTM Standards, Vol 06.01. determined throughout the operation of the bath. These parameters must be adjusted when deviations from the norm occur. 3.2 The test methods for electrocoat baths are unique, as the aqueous samples have a nonvolatile content between 8 and 25 %. Constant agitation must be present when the samples are taken and during the measurement of some of the parameters. 4. Test Methods - 4.1 Acid and Base Content--Test Methods D 4370 covers th# determination of acid and base milliequivalent content of electrocoat baths. 4.2 Electrical Conductivity--Test Method D4399 de scribes the determination of the electrical conductivity of electrocoat baths. 4.3 pH Determination--Test Method D4584 describes the measurement of the apparent pH of paints and ultrafiltrates of electrocoat baths. 4.4 Nonvolatile and Pigment Content--Test Method D 5145 covers the determination of nonvolatile and inor ganic pigment content of electrocoat baths. 5. Precision 5.1 The referenced test methods have precision limits listed. Reference to the individual standards for precision statements is recommended. 6. Keywords 6.1 electrical conductivity, nonvolatile electrocoat baths; pH; pigment content content; j The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subfect to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. Scope l.l Thi evaluating differs froi latter is ci shipping, method is random or N' 1-- measured ip of a surface, 2. Referen 2.1 AST D2091 1 D 49461 tural P 3. Termino 3.1 Defir, 3.1.1 prii forming a p< result of a p 3.2 For c Coatings Di 4. Summarj 4.1 Apiei and topped diameter of create a pres placed in a l oven for 1 h rated on the a subjective being in com 5. Significan. 5.1 The at because its ap of the coating particularly i Particularly g 238 1 This lest melh Related Coatir Subcommittee DOl Current edition 2 Annual Book < 3 Paint/Coating: boatings Technoioj DUP050297421 Designation: D 2064 - 91 iath, These m the norm ; unique, as : between 8 t when the of some of 4370 covers t content of 5 4399 deluctivity of 4 describes paints and st Method i and inor- ision limits >r precision content; Standard Test Method for Print Resistance of Architectural Paints*1 This standard is issued under the fixed designation D 2064; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. j. Scope 1.1 This test method covers an accelerated procedure for evaluating the print resistance of architectural paints. It differs from print resistance Test Method D 2091 in that the latter is concerned with lacquer finishes under packaging, shipping, and warehousing conditions, whereas this test method is concerned with decorative coatings undergoing mndom on-site pressure contact. N' 1--Printing should not be confused with blocking, which is measured in Test Method D 4946. The former relates to the indentatjon 0fa surface, and the latter, the sticking together of two surfaces. *" % Referenced Documents 2.1 ASTM Standards: D 2091 Test Method for Print Resistance of Lacquers2 D4946 Test Method for Blocking Resistance of Architec tural Paints2 3. Terminology 3.1 Definitions: 3.1.1 print resistance--the ability of a paint film to resist forming a permanent impression in a semihardened film as a result of a pressure from an object placed on it. 3.2 For additional definitions of terms, refer to Paint/ Coatings Dictionary} 4. Summary of Test Method 4.1 A piece of cheesecloth is placed on the painted surface and topped with a No. 8 rubber stopper (position smaller diameter of stopper on the cheesecloth) and a 500-g weight to create a pressure of about 0.9 psi (6.2 kPa). This assembly is placed in a 140F (60C), or other agreed upon temperature, oven for 1 h. When cooled, the resulting paint surfaces are rated on the numerical scale of 0 to 10, which corresponds to a subjective rating of an impression resulting from their being in contact with the cheesecloth. 5. Significance and Use 5.1 The ability of a coating to resist printing is important because its appearance is adversely affected if the smoothness ofthe coating film is altered by contact with another surface, particularly one with a texture. Interior paint systems, particularly gloss and semigloss on window sills and other 1 This test method is under the jurisdiction of ASTM Committee D-I on Paint hid Related Coatings and Materials and Devices and is the direct responsibility of Subcommittee DOl.42 on Architectural Finishes. Current edition approved May 15, 1991. Published July 1991. `Annual Book ofASTM Standards, Vol 06.01. 1 Paint/Coatings Dictionary, available from the Federation of Societies for Coatings Technology, Blue Bell, PA, 1978. horizontal surfaces, often have objects such as flower pots placed on them that may tend to leave a permanent impression. This tendency for a paint film to "print" is a function of the hardness of the coating, the pressure, temperature, humidity, and the duration of time that the object is in contact with the painted surface. 6. Apparatus 6.1 Conditioning Room, at 65 to 85F (18 to 29.5'C) and 40 to 60 % relative humidity. 6.2 Glass Slides, approximately 3 by 6 in. (75 by 150 mm). 6.3 Drawdown Applicator, 3-in. (75-mm) wide with a clearance of 6 mils (150 pm). 6.4 Oven, maintained at 140 + 3.5F (60 2C) or, other agreed upon temperature. 6.5 Rubber Stoppers, No. 8 (40-mm top diameter and 32-mm bottom diameter). 6.6 Cheesecloth, medium weave.4 6.7 Scissors. 6.8 Weight, 500-g. 7. Procedure 7.1 Cast the paints being tested on glass slides using a drawdown applicator with a clearance of 6 mils (150 pm), Allow the coated glass slides to dry in the conditioned room for 7 days. 7.2 Cut out approximately 1 lh by 1 Vh-in. (40 by 40-mm) pieces of cheesecloth, one piece for each slide. Use cheese cloth that is usually supplied with 4 intact layers. Do not separate the layers. 7.3 Place the test slides on a horizontal tray, painted face upward, then place one piece of cheesecloth over each slide and top with the small diameter face of a No. 8 stopper and a 500-g weight, one weight and stopper for each specimen. (Weights and stoppers should be equilibrated in the oven prior to running the test) It is recommended that control paints of known satisfactory and unsatisfactory performance be used in each test run and that the tests be run in duplicate. 7.4 Place the entire assembly in the oven and remove it after exactly 1 h. Immediately lift off the weights and stoppers without disturbing the cheesecloth and allow to cool. 7.5 After approximately Vi h, remove the cheesecloths and carefully examine the appearance of the films under neath. Note the depth and amount of cheesecloth pattern left in the paint film. If necessary examine the panel, for better 4 Idealfold bleached cotton cheesecloth, Grade 20 B, Weave 24/20, 36-in. wide, 70 yd2 available from Hermitage Industries, Inc., Camden, SC 29020, or an equivalent may be used. DU P050297422 J \ ; | f i i ?i D 2064 perception of indentations, by viewing it at a low (grazing) angle of illumination. 8. Interpretation of Results 8.1 Rate print resistance is rated on a numerical scale of 0 to 10 corresponding to a subjective rating of the degree to which the paint film has been imprinted. Record the numerical value for print resistance in accordance with the following ASTM style rating or scoring system: Numerical Rating 10 8 6 4 2 0 Qualitative Characterization (Resistance to Printing) perfect very good good fair poor very poor Quantitative Desert (Amount of Print none very slight slight moderate considerable very great 9. Report 9.1 Report the print resistance rating determined accordance with 8.1. Specify temperature used. 10. Precision 10.1 Data are unavailable for a conventional intra- and interlaboratory precision statement. However, based on actual laboratory experience, with experienced operators, the repeatability is estimated to be plus or minus one unit. The employment of common control paints with mutually agreed ratings should make it possible for interlaboratory agreement (reproducibility) to approach intralaboratory agreement (repeatability). Although numerical ratings may differ with different operators or at different times, ranking should be about the same. As in many tests the precision improves with practice. 11. Keyword 11.1 print resistance The American Society for Testing and Materials takes no posftion respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1' $ 'v i 1. pro bil saj reg 2. I 3. 3 'i | 3 10, (see p3 tun fibe datf r i 4. i4 spo is j sati rev. Pert recc Met 5. 5.L.V, sion com It if antic 240 DUP0502 97423 Designation: D 2065 - 91 ined ^ tra- and ised on tors, the nit. The nutually moratory moratory igs may ranking irecision Standard Test Method for Determination of Edge Performance of Composite Wood Products Under Surfactant Accelerated Moisture Stress1 2 This standard is issued under the fixed designation D 2065; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method is intended to serve as a means for measurement of swelling and cracking of the coated or uncoated edge of a composite wood substrate that has been subjected to wetting by a test solution containing surface active agent. 1.2 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsi bility of the user of this standard to establish appropriatet, safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D661 Test Method for Evaluating Degree of Cracking of Exterior Paints2 3. Terminology 3.1 Description of Terms Specific to This Standard: 3.1.1 crack rating--a numerical value on a scale from 1 to 10, with 10 representing no evidence of cracking of the edge (see Test Method D 661). 3.1.2 composite wood products--boards or other struc tural or decorative materials manufactured from wood fibers, flakes or strands and various resin binders consoli dated under heat, or pressure, or both. 4. Summary of Test Method 4.1 A surfactant solution is placed in a tray that contains a sponge. A preweighed and calipered panel with a coated edge is placed with the edge in contact with the surfactant saturated sponge for 2 h. The exposed panel is blotted dry, reweighed, recalipered, and inspected for edge cracking. Percentage weight and thickness changes are calculated and recorded. Edge cracking is rated in accordance,with Test Method D 661 and recorded. 5. Significance and Use 5.1 This test method provides a measure of the dimen sional stability and integrity of the coated edge, of various composite wood products under accelerated moisture stress. It is widely used as an indicator or predictor of the anticipated performance of composite wood products during 1 This lest method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DQi.52 on Factory-Coated Wood Building Products. Current edition approved May 15, 1991. Published July 1991. 2 Annual Book ofASTM Standards, Vol 06.01. exterior exposure. It may be used for developmental evalua tion ofcoatings, substrates, or both. It may also be useful for quality control or monitoring of the production of coated or uncoated composite wood products. 6. Apparatus 6.1 Wide Flat Tray or Pan, suitable to contain the required number of sponges and test boards. The sides must be high enough to safely contain at least `A in. (6 mm) of solution. 6.2 Rack or Holder, suitable to support the required number of test boards at the nominal 60 angle. 6.3 Micrometer or Vernier Caliper, of sufficient capacity for the board thickness to be measured and capable of 0.1 mm accuracy. 6.4 Balance, with sufficient capacity (typically 400 g) and 0.01 g accuracy. 6.5 Suitable Saw, for cutting of samples. 6.6 Common Household Cellulose Sponges, cut to suit able size. 7. Materials 7.1 A sufficient supply of test solution. 7.2 Appropriately identified test boards cut to proper size. 8. Hazards 8.1 When using saws, wear goggles, dust mask, and use proper machine safeguards to prevent injury. 9. Procedure 9.1 See Fig. 1. 9.2 Make the required test solution.3 Pour solution into the tray to . saturate all sponges, and allow to reach room temperature. A `A-in. (6-mm) depth of solution in the tray works well. 9.3 Cut board specimens to a suitable size. A 4 (10.2) by 5-in. (12.7-cm) size has been found to be convenient. The 4-in. (10.2-cm) dimension should be the coated edge. Prepa ration of triplicate specimens is recommended. 9.4 Measure thickness of the samples along the edge to be tested. Three measurements at 1-in. (2.54-cm) intervals (Fig. 2) are recommended for a 4-in. (10.2-cm) specimen. Record results. 9.5 Weigh the samples to the nearest 0.01 g and record. 9.6 Place boards in the tray on sponges as noted in Fig. 1. Ifcoated edges are to be tested, note that the sponges must be i Common test solutions such as 1.0 % TRITON X-100 available from Rohm and Haas Co., Independence Mall West, Philadelphia, PA 19105 or equivalent, is made using warm, {over 120*F (49C)), distilled, or deionized water. 241 DU P05 0297424 D 2065 Board t 4W (10.2 cml T BOARD 5" (12.7 cm) MEASURE XXX SPONGE FIG. 2 Specimen Dimensions narrower than the length (nominally 4 in. or 10.2 cm) of the contacting coated edges to prevent contact of the solution with the uncoated edges of the samples. Sponges 3.5-in. (9.0-cm) wide have been used successfully. For the same reason, the coated' face of the board must rest against the sponge at a 60 angle to prevent contact of the solution with the uncoated back of the board. 9.7 The test duration is 2 h. After 2 h, remove the boards and blot the edges dry with paper towels. 9.8 Observe and record changes as follows: 9.8.1 Visually inspect the edges for cracks and record the crack rating in accordance with Test Method D 661. Repeat the observation 48 h later. 9.8.2 Remeasure the thickness of the boards at the same spots measured in 4.4. Record the percent change at each spot, 9.8.3 Reweigh the boards and record the weight gain and percent weight gain, and 9.8.4 Calculate averages and standard deviations for the percent thickness change and percent weight gain. 10. Precision and Bias 10.1 The precision and bias of this test method have not been fully determined. Future round robins are planned 11. Keywords 11.1 accelerated moisture stress; detergent test; wood or composite-wood The American Society for Testing and Materials takes no position respecting, the validity of any patent rights assertedJn connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility: ' . This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have hot received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia^ PAt91031 1. Scop 1.1 T the rela visual o 1.2 T printing sions th conditio the sami of tintii color, in . N' ilar in prii D4838.2--' 1.3 T problem, bility of safety at. regulatoi 2. Refer 2.1 Ai D16 r and D387 - Pign D224< fron D274 k Whi D483; Stre E 284 Mat E 1331 Spec E 1347 Mea: Colo E 1349 ; Spec ,, 2.2 Ah 242 1 These te Paint and R Subcommitts Current o 2 Annual, 3 Annuah 4 Annual 1 5 Annual! a k. DUP0502 97425 linst the ion with e boards :cord the . Repeat the same ; at each gain and s for the have not med. .vood or I Designation: D 2066 - 91 Standard Test Methods for Relative Tinting Strength of Printing Ink Dispersions1 This standard is issued under the fixed designation D 2066; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. \. Scope 1.1 These test methods cover procedures for determining the relative tinting strength of printing ink dispersions by yisual or instrumental evaluation. 1.2 These test methods are applicable to paste-type printing inks, flushed pigments, and other pigment disper sions that are essentially nonvolatile under ordinary room conditions and for which there is a wet reference standard of the same pigmentation and consistency. With proper choice of tinting base, they are applicable to dispersions of any color, including black and white. N' 1--The instrumental procedures for tinting strength are sim ilar in principle to those described in Test Methods D 387, D 2745, and D4838.2'' 1.3 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsi bility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products4 D387 Test Method for Color and Strength of Colored Pigments with a Mechanical Muller2 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates3 D 2745 Test Method for Instrumental Tinting Strength of White Pigments2 D4838 Test Method for Determining the Relative Tinting Strength of Chromatic Paints3 E 284 Definitions of Terms Relating to Appearance of Materials5 * E 1331 Test Method for Reflectance Factor and Color by Spectrophotometry Using Hemispherical Geometry5 E 1347 Test Method for Color and Color-Difference Measurement of Object-Color by Tristimulus (Filter) Colorimetry5 E 1349 Test Method for Reflectance Factor and Color by Spectrophotometry Using Bidirectional Geometry5 2.2 ANSI Standards: PH 2.17 Geometric Conditions for Reflection Density6 PH 2.18 Spectral Conditions for the Measurement of Optical Density6 PH 2.30 Viewing Conditions for Graphic Arts and Photog raphy--Color Prints, Transparencies and Photome chanical Reproductions6 3. Terminology 3.1 Definitions relating to color attributes and color differences are covered in Terminology D 16 and E 284. 3.2 Descriptions ofTerms Specific to This Standard: 3.2.1 tinting strength--the ability of a material to impart its color to a standard base; the reciprocal of the relative concentration required to match the reference material in a standard base. 3.2.2 masstone (or masscolor)--the color of a material that is thick enough to mask any background. 3.2.3 undertone (or undercolor)--the color of a thin film of a material. 4. Summary of Test Methods 4.1 Thin and thick films of the standard and unknown dispersions are drawn down in juxtaposition on bond and on coated paper, Visual evaluation ofthe relative undertone and masstone provides a check on color equivalency. 4.2 The standard and unknown dispersions are each reduced to the same concentration in a suitable tinting base. Thick wet drawdowns of the two tints are evaluated for tinting strength by Test Methods A or B. 4.2.1 Test Method A--Visual Evaluation: If the strength of the tints isjudged unequal, aliquots of the stronger tint are further reduced until equivalence is obtained. The tinting strength of the unknown dispersion is calculated from the weight of extra tinting base added per unit weight of the stronger tint. 4.2.2 Test Method B--Instrumented Evaluation: Reflec tance measurements are made on thick wet films of the original tints. The tinting strength ofthe unknown dispersion is calculated according to the Kubelka-Munk equation. 4.3 Preparation of a confirming tint is recommended as an unbiased method of verification. The preferred approach is to prepare a new tint of the unknown at a concentration calculated to match the standard tint. 1 These test methods are under the jurisdiction of ASTM Committee D-I on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D1.S6 on Printing Inks. Current edition approved May 15, 1991. Published July 1991. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vol 06.01. 1 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 5 Annual Book ofASTM Standards, Vol 14.02. 5. Significance and Use 5.1 Tinting strength is an essential property of printing ink dispersions. Although test results on wet drawdowns and * Available from American National Standards Institute, 13th Floor, 11 W 42nd St., New York, NY 10036. 243 DUP050297426 # D 2066 tints do not guarantee equivalency of dry printed ink flints, they provide useful parameters for quality assurance of established formulations, gaging relative degree of dispersion, and estimating the color value of colorants from different batches, sources, or grades. 6. Apparatus 6.1 Laboratory Balance, sensitive to at least 1.0 mg, preferably 0.1 mg. 6.2 Spatulas, (2) with flexible blades 80 to 120 mm in length (for weighing and mixing). 6.3 Mixing Surface, such as a glass or similar slab fixed to a work bench. 6.4 Putty Knife, with an 80-120 mm wide blade having a smooth straight edge (for use as a drawdown blade). 6.5 Standard Daylight, preferably a D50 light source conforming to ANSI Standard PH 2.30. 6.6 Reflectance Measuring Instrument, (for instrumental evaluation). Unless otherwise agreed upon, the instrument shall be a spectrophotometer with hemispherical (integrating-sphere) geometry conforming to Test Method E 1331, a spectrophotometer with bidirectional (45/0 or 0/45) geom etry conforming to Test Method E 1349, or a tristimulus (filter) colorimeter with either geometry conforming to Test Method E 1347. Alternatively, a reflection densitometer conforming to ANSI Standard PH 2.17 and having a set of Status T or Status E filters7 (see 12.3.2), conforming to ANSI Standard 2.18 may be used for certain colors. N' 2--The filter systems in typical densitometers are suitable only for use with black, white, and the three process colors {yellow, magenta and cyan). Instrumental evaluation of other colors requires a spectrophotometer or a colorimeter. 7. Materials 7.1 Reference (Standard) Dispersion, having the same pigmentation and consistency as the test (unknown) disper sion. 7.2 Tinting Base, as agreed upon between the producer and user, consisting of a suitable pigment well dispersed in a vehicle that is compatible with the vehicle in the test dispersion. The consistency of the base should not be appreciably lower than that of the test dispersioii. Driers are not generally used because they may affect the color of the base and corresponding tints. 7.2.1 White Base,8 for testing colored and black disper sions. A suitable white base may contain by weight 60 % of either zinc oxide or titanium dioxide and 40 % vehicle. 7.2.2 Black Base, for testing white dispersions. A suitable black base may contain by weight 4 % black pigment (preferably non-flocculating), 43 % precipitated calcium car bonate, and 53 % vehicle. Alternatively,, a neutral black nondiying printing ink such as a news ink. 7.2.3 Dark Blue Base (optional), for visual testing ofwhite dispersions. A suitable dark blue base may contain by weight 7 Status T filters are available in the USA, Status E in other countries. The major difference is in the peak transmission of the blue filter. 8 A spectrophotometrically controlled universal white bleach, containing by weight 60 % zinc oxide (Florence White Seal) and 40 % Hercolyn-D plasticizer, is available from National Printing Ink Research Institute (NPIRI), Lehigh Univer sity, Sinclair Laboratory 7, Bethlehem, PA 18015. 42 % ultramarine blue, 18 % precipitated calcium carbonate, the hue, Iand 40 % vehicle. 7.2.4 Light Blue Base (optional), for visual testing of yellow dispersions. A suitable light blue base may contain by weight 1 % phthalocyanine blue dispersion and 99 % white ties of tJ dispersiot S over whit j the black base. f as the rel N' 3--Mixtures of a light blue base with yellow samples produce green tints, differences between which are more easily detected by eye than are mixtures of white and yellow. However, false results may be obtained. The use ofa blue base is not recommended for visual tests on greenish-yellow colorants and is not permitted for instrumental evaluation of any yellow coloram. 7.3 Weighing Substrate, nonabsorbent, such as skin paper9 or small glass plates ca 75 to 100 mm square. 7.4 Drawdown Substrates, one consisting of white bond paper at least 50-mm wide and 150-mm long with a black bar at least 20-mm wide imprinted across the short dimen sion about half way down the length of the sheet, and a second one consisting of white coated paper.10 7.5 Microscope Cover Glasses11 (optional, for instrumental measurements), made of finest optical glass, 50 by 4S | 9.4 Re I coated p.| relative u ! evaluatio N' 4 ; dispersion: drawdown ! relative hu i in 11.6). N' - -5 ! cantly diffi tested by assessment ments act calculating ance with mm, 0.13- to 0.17-mm thick. 7.6 Standard Spacer (optional, for instrumental measure, ments), such as cardstock the same size as the cover glass described in 7.5, about 1-mm thick, with a 35-mm diameter hole. 10. Pref < .< ; tested (s< signs of: necessar 8. Sampling 8.1 These test methods do not include a method for preparation of dispersions. If colorants from different batches or sources are being evaluated, it is important that the standard and unknown samples be dispersed either in the identical manner or to the maximum degree, as agreed upon between the producer and the user. 8.2 Carefully select a dispersed sample that is free of skin and other contamination and representative of the lot being evaluated. Transfer to a clean container, protect with skis paper, close and seal. and mix used for 10.2 ' guidelim amount need no to at lea by the d weight, specime be add 10.3 ' weighin 9. Evaluation of Masstone and Undertone for Relative Color stirring 9.1 Using the bond paper with the black bar, place small surface portions of the standard and unknown dispersions close further together, but not touching, in the center at one end of the sheet in the long dimension. TABLE 9.2 Place the blade of the drawdown knife behind the j pastes and, using heavy pressure, draw down a thin film of i the pastes in juxtaposition. When the middle of the black bar j is reached, raise the blade slightly and draw down the j remaining pastes in a layer sufficiently thick that the black ! bar is not visible. Remove excess material. ] 9.3 Immediately examine the drawdowns under the j standard D50 light or other agreed upon light source. Judge T Dl; Rush or o Process o baked or l color Titanium c with Ian _ with oat 9 Skin paper available from NAV Pack, 18 Monterey Lane, Englishtown. W 07726 or equivalent, has been found suitable for this purpose. 10 Bond paper with a black bar (Form 3NT-4) available from The Leneta Gh P.O. Box 86, Hohokus, NJ 07423 or equivalent, has been found suitable forth* purpose. 11 Microscope cover glasses available from Fisher Scientific Co. (catalogue 12-S45H) or other scientific supply houses have been found suitable forth* purpose. * In NF a guide, it cneentra "Mate a factor ci c Use 3Pectropn "Fort 244 DUP050297427 arbonat'e, esting of ontain by % white es produce ted by eye Its may be lal tests on itai evalua- as skin e. lite bond i a black 1 dimen;t, and a r instru50 by 45 measure>ver glass diameter :thod for different tant that tier in the eed upon ;e of skin lot being vith skin re Color :e small is close i of the tind the n film of black bar iown the the black nder the ce. Judge lishtown, NJ Leneta Co., table for this :atalogue no. able for this D 2066 jg hue, depth, cleanliness, transparency and other proper^ of the unknown dispersion relative to the standard jjspersion. Record qualitative observations of the thin film flVer white paper as the relative undertone, the thin film over jjjg black bar as the relative transparency, and the thick film the relative masstone. 9.4 Repeat 9.1 and make a tight drawdown on a sheet of goated paper. Make an immediate visual judgment of the (glative undertone. Include relative gloss and bronzing in the gvaluation. fjoTE 4--When the consistencies of the standard and unknown (jispersions are significantly different, the film thicknesses of the tight ^wdowns may not be comparable. In such cases, judgments regarding Native hue should be reserved until the tints are examined (see Note 8 ja ll.fi)* fjOTE 5--If the hue or cleanliness of the test dispersion i'S significatttly different from the standard dispersion, tinting strength cannot be tested by the procedures covered in this test method. A numerical assessment of such systems may be obtained by making color measure ments according to Test Methods E 1331, E 1347, or E 1349 and calculating color differences by the 1976 CIELAB equations in accord ance with Test Method D 2244. 10. Preparation of Tints 10.1 Select a tinting base appropriate to the sample being tested (see 7.2). Examine the base for uniformity. If there are signs of separation or settling, stir thoroughly in container. If necessary, transfer the quantity required for testing to a slab and mix to ensure that the same composition of base will be used for both the standard and the unknown samples. 10.2 Tare or counterbalance a weighing substrate. Using guidelines suggested in Table 1, weigh out the desired amount ofthe standard dispersion. The quantity of specimen need not be exactly as listed in Table 1 but must be weighed to at least three significant figures. Divide the actual weight by the desired decimal concentration to obtain the total tint weight. The difference between the total weight and the specimen weight represents the weight of bleaching base to be added. 10.3 Gently mix the specimen and tinting base on the weighing substrate until the tint is uniform. Use a circular stirring motion, periodically scraping all material from the surface of the substrate. Do not use so much energy that further dispersion will result. If necessary, transfer all mate- TABLE 1 Suggested Tint Concentrations for Strength Testing of Printing Ink Dispersions4 Type ol Dispersion Dispersion Ratio Concentra Disper tion in Tint sion Content of Tint,ao g Disper- Tinting sion Base TotaJ Flush or concentrate 0.01 1:99 0.05 4.95 5.0 Process color ink 0.02 1:49 0.10 4.90 5.0 Laked or low strength 0.05 1:19 0.25 4.75 5.0 color Titanium dioxide with lamp black base 0.85 6:1 4.25 0.75 5*0 with carbon black base 0.98 49:1 4.90 0.10 5.0 4 In NPIRI Universal Bleaching Base except where noted; Figures are given as a guide. It is recommended that standard batches be checked Erst to establish tint concentrations that give proper lightness levels. s Materials should be weighed to three significant figures. Increase weights by a (actor contingent on the balance sensitivity. "Use double the quantity for instrumental tinting strength conducted by spectrophotometry and confirmed by aliquot reduction. 0 For white dispersions, weigh tinting base first. rial to a glass slab and continue mixing with a gentle scraping and stirring motion until a uniform color with no specks or streaks is achieved. With a clean putty knife, push the tint to one side of the slab. Clean the putty knife and remainder of the slab. N' 6--With flushes and other high viscosity dispersions, it is recommended that the tinting base be mixed into the specimen in small increments. 10.4 Repeat 10.2 and 10.3 with the unknown dispersion. Be sure the specimen concentration in the tint and the type of tinting base are identical to that used for the standard dispersion. 10.5 If there will be a delay in the evaluation process, transfer the tints to small clean containers and label appro priately. Always gently restir immediately before subsequent use in order to minimize problems of flooding or floating. TEST METHOD A--TINTING STRENGTH BY VISUAL EVALUATION 11. Procedure 11.1 Using separate ink knives, gently stir the standard and the test tints. Place a small quantity of each tint close together, but not touching, at one end of a small glass plate or other drawdown substrate. Hold the drawdown knife at a low angle (5 to 15from horizontal) and, using light pressure, draw down the tints in juxtaposition. The two films must be in contact with each other, smooth, and sufficiently thick so as to mask any background. 11.2 Immediately examine the drawdowns under the standard light If the two tints appear equal, record the tinting strength of the unknown as 100 %. If the tints are unequal in strength, estimate the strength difference between the stronger and weaker color either from experience or from instrumental measurements (see Eq 4a or 4b in 13.2.2). N' 7--With colored and black samples, the stronger tint will be darker. With white samples, the stronger tint will be lighter. 11.3 Weigh to three significant figures an aliquot of about 1 g (or a quantity representing about 10 to 20 %) of the stronger tint Multiply the exact weight by the estimated strength difference in decimal units; add tinting base accord ingly. For example, for an estimated 10 % difference, add 0.10 g base/g aliquot of the stronger tint. 11.4 Gently mix the adjusted tint until uniform. Gently remix the original tint of the weaker dispersion, make a thick drawdown versus the adjusted tint as in 11.1, and examine as in 11.2.. 11.5 If the drawdowns are still unequal, discard the adjusted tint. Weigh out a new aliquot of the stronger tint and add more or less tinting base than in 11.3. 11.6 Repeat 11.3 and 11.4 until the drawdowns show that the adjusted tint equals the strength of the lighter tint. When equivalency is obtained, record whether the standard or unknown tint was stronger, the weight of the final aliquot, and the weight of added tinting base. N' 8--Ifthere is a difference in color between the unknown and standard dispersions, a situation will result wherein, as dilution progresses, feedarker- tint wiferevert to fee lighter tint without obtaining a match. In such cases, this method cannot be used (see Note 5). 11.7 Compute the strength of the unknown dispersion (u) 245 DUP050297428 D2066 as a percentage of a standard dispersion(s) as follows: 1 + {bfa)u TSW % x 100 1 + (.b/a). (1) where: TSU = tinting strength of the unknown dispersion, b = weight of extra tinting base added to an aliquot of the stronger tint to obtain equivalence, g, and a = weight of the aliquot, g. The term b/a represents the strength difference between the stronger and weaker colorant. For the weaker dispersion, b/a = 0 and drops out of Eq 1. When the unknown dispersion is stronger, Eq 1 reduces to: TSU, % = 1 + (b/a)u x 100 (la) When the standard dispersion is stronger, Eq 1 reduces to: TSU, % =------------ x 100 1 + (b/a). (lb) N' 9--Tinting strength is always expressed as a decimal or a percentage of the unknown relative to the standard. The practice of expressing results as a strength difference may lead to erroneous calculations of the replacement concentration. See Eq 3 in 13.1. 11.8 Since replication of visual tinting strength tests inherently suffers from bias, prepare a confirming tint in accordance with the procedure given in 13.1. TEST METHOD B--TINTING STRENGTH BY INSTRUMENTAL EVALUATION 12. Procedure 12.1 Set the instrument for the large area of view or illumination and standardize in accordance with Test Methods E 1331, E 1347, or E 1349, or, in the case of a densitometer, the manufacturer's instructions. If it is the intent to make measurements directly on wet tints, it may be useful to protect the instrument with a material such as plastic wrap with the porthole cut out. 12.2 Gently remix the standard tint prepared in Section 10. Place a sufficient quantity on a small glass plate or other rigid surface so that the material is at least 30 to 35 mm in diameter and thick enough to mask any background. Alter natively, use a standard spacer (see 7.6) to prepare a thick sandwich between two microscope cover glasses. 12.3 Measure the reflectance factor in one ofthe following manners: 12.3.1 Spectrophotometer: Following the procedure given in Test Method E 1331 or E 1349, quickly mountthe tint on the porthole of the spectrophotometer and, within or at 45 s, measure the reflectance factor between 420 and 680 nm. If hemispherical geometry is used, the specular component may be either included or excluded, as long as the same condition is consistently used. Make a minimum of two measurements, moving or rotating the specimen between runs. Record the spectral reflectance factor in decimal units at the wavelength ofmaximum absorption (minimum reflec tance) and compute the mean. 12.3.2 Densitometer: If the tint involves black, white or a process color, select the filter having the appropriate Status T or Status E response in accordance with ANSI Standard PH 2.18. The peak transmission of The visual response filter should be at 555 nm for blacks and whites; of the blue filter, at 460 nm (Status T) or 440 nm (Status E) for process yellows; of the green filter, at 530 nm for magentas; of the red filter, at 600 nm for cyans. Make measurements as in 12.3.1 at two or three different locations. If the readout is density, convert to the reflectance factor as follows: R = 10--. s ; i If the readout is percent reflectance, record in decimal units, 12.4 Alternatively, measure the CIE tristimulus values of the specimen on a spectrophotometer in accordance with Test Method E 1331 or Test Method E 1349 or on a tristimulus colorimeter in accordance with Test Method E 1347. Make the measurements as in 12.3.1. If hemispher ical geometry is used, the specular component may be either included or excluded as long as the same condition is consistently used. The tristimulus values may be based on either the CIE 1964 (10`) supplementary standard observer and standard illuminant D65 or the CIE 1931 (2) standard observer and standard illuminant C, as long as the same basis is consistently used. Record in decimal units the lowest appropriate value, for example, X with blue colon, Y with -reds, blacks, and whites, or Z with yellows. 12.5 Repeat 12.2 and 12.3 or 12.4 with the unknown tint. 12.6 Calculate the tinting strength of the unknown disper sion according to the Kubelka-Munk equation as follows: : [(1 TSU, x 100 [(I - RJ2/2RJs (2) where: = spectral reflectance factor, expressed as a decimal fraction, of an infinitely thick layer of material (at the wavelength of maximum absorption), or, by mutual agreement, an appropriate tristimulus value. N' 10--If the tint represents a white pigment, use Eq 2 in the inverted form. N' 11--The term ((1 - J?J2/2RJ represents KjS of the colorant, where K is the absorption coefficient and S is the scattering coefficient, both of which are specific to a colorant. Therefore, if the pigmentation in the unknown dispersion is different from that in the standard dispersion, that is, the dispersions are metameric, Eq 2 no longer applies, The equation is also reported to work best when the reflectance factor or tristimulus value of the tints used is about 0.40 and the tinting strength ofthe unknown is within 10 % of the standard. l ! \ f 12.7 If the tinting strength result for the unknown is not within 10 % of the standard, reduce an aliquot of the stronger tint by the procedure given in 13.2. Remeasure the adjusted tint and calculate a new tinting strength value (see 13.2.5). 12.8 Prepare a confirming tint (see 13.1) if the original tinting strength value was not within 10 % of the standard (see 13.1 or 13.2 ifwithin 10 %). | S | j f j 13. Preparation of Confirming Tint f 13.1 Replacement Concentration: 13.1.1 In, this method of confirmation, a new tint of the unknown dispersion is prepared at a concentration calcu- lated to match the standard tint. 13.1.2 Compute the replacement concentration, also called color value, as follows: C,, = CJTSU ' (3) \ \ j ; | where: j Cu Cs TSU 13. simik C,,to total: base i 13. dispei If the for th 13. weigh and s' 13. colon Cu an of otl Cu) a value 13.. 13.) tintin differs aliquc 13..' range) strong then: If the than 13. Mult; bleac unifo 13. proce 13versus Failur weigh: equati until i streng 13.1 the ad adjust tinting correc strengdecim 14. R, 14.1 246 DUP050297429 s; of the ItS LS ^ adout is al units, 'alues of ice with >r on a Method uispherae either lition is >ased on observer standard me basis e lowest . Y with )wn tint, n disperillows: (2) decimal al (at the ' mutual 1 2 in the 2 colorant, efficient, mentation standard ;er applies, e factor or g strength n is not of the sure the due (see original standard nt of the an calcu- on, also D 2066 C = concentration of the unknown dispersion required " to match the standard dispersion, q = concentration of the standard dispersion in the 5 original tint prepared in 10.2, and ^ = tinting strength result for the known dispersion in " decimal units. 13.1.3 Weigh out a quantity of the unknown dispersion similar to that employed in 10.2. Divide the actual weight by q to obtain the total tint weight. The difference between the total and the specimen weight represents the weight oftinting base to be added. Mix as in 10.3. 13.1.4 Gently remix the original tint of the standard dispersion- Make a thick drawdown of both tints as in 11.1. If the two tints match, the tinting strength result computed for the unknown dispersion is correct. 13.1.5 Failure of the two tints to match suggests a weighing error or inadequate mixing of .the tints. Clean up and start over from Section 10. 13.1.6 Use Eq 3 to compute the color/money/value of a colorant from different sources or grades (optional). Multiply C and Cs by their respective unit costs. Add to each the costs of other components in a formulation, represented by (1 -- Ca) and (1 - Cs). The lower total cost figure is the better value. 13.2 Reduction of the Stronger Tint: 13.2.1 In this method of confirmation, the instrumental tinting strength result is used to calculate the strength difference between the stronger and weaker dispersion. An aliquot of the stronger tint is reduced accordingly. 13.2.2 Compute the strength difference, bja by re-ar rangement of Eq la or lb. If the test dispersion is the stronger, that is, TSU in decimal units is greater than 1.0 then: (h/a)u = TSU - 1 (4a) If the standard dispersion is the stronger, that is, TSU is less than 1.0 then: (A/)s = (i/ra,,)-1 (4b> 13.2.3 Weigh out an aliquot of the stronger tint as in 11.3. Multiply the exact weight by bja to obtain the weight of bleaching base to be added. Mix the adjusted tint until uniform. 13.2.4 Evaluate the adjusted tint by either ofthe following procedures: 13.2.4.1 Visual Evaluation-Draw down the adjusted tint versus the original tint of the weaker color as in 11.1.4. Failure to obtain equivalency on the first cut may suggest a weighing error or the inapplicability of the Kubelka-Munk equation (Eq 2), or both. If necessary, reduce a new aliquot until equivalency is obtained. Calculate the correct tinting strength according to Eq la or lb. 13.2.4.2 Instrumental Evaluation--Prepare a thick film of foe adjusted tint, remeasure the reflectance, and calculate the adjusted tinting strength by Eq 2. If 100%, the original tinting strength value is correct. If not 100 %, compute the correct tinting strength by multiplying the original tinting strength percentage by the adjusted tinting strength in decimal units. 14.1.1 The type and identification of the test dispersion, the reference standard dispeision, and the nature of the tinting base, 14.1.2 The results of the visual evaluation of the relative color difference (masstone and undertone) of the drawdowns on bond and coated paper, 14.1.3 The relative tinting strength and the method by which it was determined (visual or instrumental). If the instrumental method was used, the manufacturer and type of instrument, the geometry (including for hemispherical geom etry whether the specular component was included or excluded) and, if used, the basis for the calculation of tristimulus values, 14.1.4 The method, if any, by which the tinting strength result was confirmed, and 14.1.5 Any deviation, by agreement or otherwise, from the procedures given in these test methods. 15* Precision and Bias 15.1 Precision: 15.1.1 An interlaboratory study of these test methods was conducted in which 3 sets of process color printing inks ranging in tinting strength from 75 to 85 % were tested by operators in 6 different laboratories. The tests were con ducted as blind duplicates on each of 2 days. In addition to visually evaluated tinting strength, the same reductions were measured spectrophotometricaliy or densitometrically, or both. The estimated standard deviations and the degrees of freedom are given in Table 2. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 15.1.1.1 Repeatability--Two results obtained by the same operator on different days should be considered suspect if they differ by more than the maximum allowable difference indicated in Table 2. 15.1.1.2 Reproducibility--Two results, each the mean of results obtained on different days by operators in different laboratories, should be considered suspect if they differ by more than the maximum allowable difference indicated in Table 2. 15.2 Bias--The tinting strength results obtained in the interlaboratory study of these test methods were higher than the formulated values by the amounts shown in Table 3. 16. Keywords 16.1 colorimeter; densitometer; Kubelka-Munk equation; pigment dispersions; printing inks; relative tinting strength; spectrophotometer TABLE 2 Precision of Tinting Strength Determinations Method of Evaluation Standard Deviation, % absolute Degrees of Freedom Maximum Alowabte Difference, % absolute Visual Spectrophotometer Densitometer Repeatability 1.3 12 3.7 1.8 8 5.0 3.6 10 to.t Reproducibility Visual Spectrophotometer Densitometer 2.8 12 8.0 1.7 8 4.7 4.8 12 13.4 | 247 DUP050297430 D 2066 TABLE 3 Accuracy ot Tinting Strength Results Method of Evaluation Difference Between Overall Mean Test Results and Formulated Tinting Strength, % absolute Visual Spectrophotometer Densitometer +0.73 +3.87 +1.90 A If the unknowns had been stronger than the standard, the plus signs would be minus signs. e Values are based on the original tints, not on adjusted tints as recommended in 12.6. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not revised, either reapproved or withdrawn. Tour comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Rfce St., Philadelphia, PA 19103. ! i P ,\ |\ Is 1 ,r ______ ___ ______________ __ _______ _ 248 DUP050297431 Designation: D 2091 - 88 Standard Test Method for Print Resistance of Lacquers1 This standard is issued under the fixed designation D 2091; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 6211 of Federal Test Method Standard No. 141. Consult theDoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 This test method covers the resistance ofdried lacquer films to imprinting. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the-applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 ' D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of NonconductiveCoatings Ap plied to a Nonferrous Base2 f 2.2 U.S. Federal Specifications: /. CCC-C-419(f) Cloth, Duck, Cotton, Unbleached, Plied? CCC-C-440(e) Cloth, Cheesecloth, Bleached and Un bleached3 .r 3. Summary of Test Method 3.1 A weight presses a piece of fabric against the test surface. The surface is then examined and changes in appearance of the test surface are reported. 4. Significance and Use 4.1 An unsatisfactory appearance can result from pressure deformation of a film inherently too soft or containing residual solvent. This test method is primarily used to evaluate the resistance of a lacquer finish to printing under the conditions of packaging, shipping, and warehousing. 5. Apparatus and Materials 5.1 Test Panels--A plane surface consisting of wood, metal, paper supported on plate glass, plastic, or other surface with an area at least 100 % greater than the base of the- weight. The planeness, smoothness, and composition should be agreed upon by the purchaser and the seller. 5.2 Imprinting Fabric, 8-oz Army duck, Type III, con forming to Fed. Spec. CCC-C-419(f) or cheesecloth, Type I, conforming to Federal Specification CCC-C-440(e). N' --With the cheesecloth only, use a pad of nonwoveu felt cloth at least 0.05 in. (1.3 mm) thick, weighing 7 oz/yd2 (0.24 kg/m2) and larger than the plane end of the weight. 5.3 Weights, consisting of metal cylinders cut from standard stock 2 in. (51 mm) in diameter, with plane ends perpendicular to the axis, and ofa length to give a pressure of xh or 1 lb/in 2 (3.5 or 7.0 kPa). 5.4 Automatic Application Equipment, {Optional), as de scribed in Test Methods D 823. 5.5 Film Thickness Measuring Apparatus, as described in Test Methods D 1005, D 1186, and D 1400. 6. Preparation of Test Specimen 6.1 Single Coats--Prepare a specimen for test by applying the test lacquer to a panel with a film applicator or other specified' method, as described in Test Methods D 823, to give a specified film thickness to be stated in the result. In the absence of a specified dry film thickness, 1 0.1 mil (25 3 pm) is recommended. 6.2 Multiple Coats--Use the finish system as agreed upon between the purchaser and the seller. In the absence of a specified dry film thickness, 3 0.3 mils (75 8 pm) are recommended. 6.3 Conditioning--Allow to dry as agreed upon between the purchaser and the seller, but run the test within 48 h after coating. In the absence of a specified drying schedule, a period of 24 h at 73.5 3.5F (23 2C) and a relative humidity of 50 5 % is recommended. 5 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D 01.55 on Factory-Applied Coatings on Preformed Products. Current edition approved March 25, 1988. Published September 1988. Origi nally published as D 2091 -62 T. Last previous edition D 2091 - 87, 2 Annual Book ofASTM Standards, Vol 06.01. 3 Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 7. Procedure 7.1 Place over a uniform area of the specimen either a smooth piece of duck cloth or a piece of cheesecloth with a felt pad cushion. Place one or more weights, each on top of the other, on the duck or cheesecloth and pad and maintain the weight in compliance with one of the following test conditions: 249 DUP050297432 # D 2091 \ 7.1.1 At 73.5 3.5F (23 2C) and 50 5 % relative humidity for an 18-h period, 7.1.2 At 120F (50C) for a 4-h period, or 7.1.3 At 140*F (60C) for a 4-h period. 7.2 After the specified time, remove the weight, pad, and fabric. Remove lint and dust from the panel with a dean air stream. Examine the spedmen immediately under bright, diffused illumination for impression of the fabric into the lacquered surface and compare to photographic standards (Fig. 1). 8. Report 8.1 Report the following information: 8.1.1 Surface involved, 8.1.2 Drying schedule, 8.1.3 Film thickness, 8.1.4 Weight used, 8.1.5 Test temperature used, time, and 8.1.6 Conditions of test other than those primarily speci fied in this test method. 9. Precision 9.1 Results varying by more than 1 of print should be suspect, either with the same or different operators. 1! (a) Heavy pa eit co m m A] at ac th ap ap 2. I (b) Medium FIG. 1 Print Resistance (c) Slight The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of tha validity of any such patent rights, and the risk of Infringement of. such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feeI thet your comments have not received a fair hearing you'Should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. 250 am 3. Pi so ne cc Re DO 701 vie DUP0502 97433 Designation: D 2092 - 86 ly specilould be Standard Practice for Preparation of Zinc-Coated (Galvanized) Steel Surfaces for Painting1 This standard is issued under the fixed designation D 2092; the number immediately following the designation indicates the year of originai adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. j. Scope 1.1 This practice describes six methods of preparation for painting new zinc-coated (galvanized.) surfaces produced by either the hot-dip method or by electroplating. This practice covers surfaces that have not been treated previously at the mill to provide temporary protection against staining by moisture other than by easily removed protective oils.-(see Appendix XI). 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 U.S. Federal Specification: TT-P-641 Primer Coating, Zinc Dust Oxide (for Galva nized Surfaces)2 2.2 U.S. Military Specification: DoD-P-15328 Primer (Wash) Pretreatment (Formula No. 117 for Metals)2 2.3 Canadian Standard: CGSB, l-GP-198 Primer, Cementitious for Galvanized Surfaces3 2.4 Steel Structures Painting Council Specification: Paint No. 27 Basic Zinc Chromate-Vinyl Butyrol Wash Primer4 3. Summary of Practice 3.1 This practice describes methods of preparation that provide galvanized surfaces suitable for painting, specifically so that an applied coating system can develop the adhesion necessary for satisfactory service life. 3.2 Six methods of surface preparation (Note 1) are covered as follows: 3.2.1 Method A--Crystalline Zinc Phosphate Treatment. 1 This practice is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.46 on Industrial Protective Coatings. Current edition approved Sept. 26, 1986. Published November 1986. 2 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 3 Available from Canadian Government Publishing Center, Supply and Ser vices, Ottawa, Ontario Ki A OS9 Canada. 4 Available from Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, PA 15213. 3.2.2 Method B--Chromate Treatment. 3.2.3 Method C--Aqueous Chromic-Organic Treatment. 3.2.4 Method D--Acid-Bound Resinous Treatment. 3.2.5 Method E--Annealing Heat Treatments. 3.2.6 Method F--Amorphous Complex-Oxide Treat ment. N' 1--Materials employed in these methods of treatment are available from a number of sources as proprietary compounds or methods. Selection may be made from available sources. 3.3 Variations in surface preparation produce end condi tions that differ and that do not necessarily yield identical results when paints are applied. Service conditions will dictate the type of surface preparation to be selected, although the quality produced by any individual method may vary with different zinc coatings. 3.4 Galvanized. surfaces are treated by using various methods and apparatus; satisfactory application may be made at the following locations: Method A Method B Method C Method D Method E Method F Mill Plant Field Y YY YY YY Y YY Y YY 3.5 This practice does not describe the cleaning necessary to provide a zinc-coated (galvanized) surface suitable for the application of the treatments. Many cleaning methods are applicable and should be agreed upon between the purchaser and the supplier. N ' 2--Most producers ofzinc-coated (galvanized) steel sheets and coils have adopted the practice of applying an inhibitor to the zinc surface to give temporary protection against staining by moisture during shipping or storage. Some of these inhibitors will interfere with proper reaction of most of the treatments described in these methods, and an unsatisfactory surface for painting will result. It is strongly recom mended that the purchaser consult the supplier of the chemical treatment to be used as to the suitability of the zinc surfaces for treatment by any of these methods (see Appendix X2). 4. Significance and Use 4.1 This practice describes procedures that can be used to prepare new zinc-coated surfaces for painting and improve the bond of paint to the zinc surface. 5. Processes 5.1 Method A, Crystalline Zinc Phosphate Treatment-- This conversion-coating method consists of reacting the zinc surface in a zinc acid phosphate solution containing oxi- 251 DUP05 02 97434 # D 2092 living agents and other salts for accelerating the coating action. The zinc surface is converted to a crystalline phos phate coating of the proper texture to inhibit corrosion and increase the adherence and durability of the paint film. Such treatments are recommended for product finishes and may be carried out by immersion, spray, or brush application. 5.2 Method B, Chromate Treatment--This treatment consists of a dip or spray with a dilute solution of a mixture of chromium trioxide and other acids, with the proper accelerator, for a period from 5 to 30 s at room temperature to 130F (55C) to provide a thin amorphous chromate coating that increases corrosion resistance and paint adhe sion. 5.3 Method C, Aqueous Chromic-Organic Treatments-- Certain water-soluble resins, when properly formulated with chromium compounds, may be applied to zinc surfaces by roller coat or other suitable means, such as dip and squeegee rolls. This may be done over a wide temperature range provided the film is properly baked or cured, or both, as required by the paint system to be applied. The resultant coating provides a corrosion-resistant film that increases the adhesion of applied paint films. 5.4 Method D, Acid-Bound Resinous Treatment (Vinyl Wash Primer) (See DoD-P-15328 and SSPC-Paint No. 27)--This surface treatment is based on the application ofan acid-bound resinous film of approximately 0,3 to 0.5 mil (8 to 13 pm) thickness. The treatment is based on three primary components: a hydroxyl-containing resin, a pigment capable of reacting with die resin and an acid, and an acid capable of insolubilizing the resin by reacting with the resin, the pigment, and the zinc surface. The film is usually applied by spray, but may be applied by brash, dip, or roller coater. Under normal conditions it will dry sufficiently for recoating within 30 min, and within 8 h it will not be softened by organic solvents commonly used in paint coatings. The film has good adhesion to the metal substrate and promotes good adhesion of most subsequent organic coatings to itself. Two types of this treatment are available: (2) two-package mate rial to be used the day it is mixed and (2) one-package material that has package stability and does not require daily preparation. N' 3--It may be difficult to control the dry film thickness within the parameters of this specification when applied by brush, roller, or dip coater. 5.5 Method E, Annealing Heat Treatments--Under the controlled conditions obtainable in a mill, hot-dip galvanized surfaces may be converted and alloyed with the base metal to change the surface character of the zinc coating and make it more` receptive to paint. This surface can be further im' proved by treating in accordance with Methods A, B, C, or D. 5.6 Method F, Amorphous Complex-Oxide Treatment-- This surface treatment method consists of reacting the zinc surface in an alkaline solution containing heavy metal ions for a period of 5 to 30 s at 115 to 160F (45 to 70C). The surface ofthe zinc is converted to a nonmetallic, amorphous, complex-oxide coating that inhibits corrosion and increases the adhesion and durability of paint finishes. The treatment can be carried out by immersion or spray application. dipheny used to the treai X2.5 X2.5. powder ethanol. X2.5. 40 mL water. X2.5. alcohol X2.5. Appendixes (Nonmandatory Information) XI. CLEANING OF ZINC SURFACES X1.1 When zinc surfaces treated by Methods A through F have been soiled in fabrication, they should be cleaned before finishing. Alkali and acid cleaners should not be used without consulting the supplier of the treatment Organic solvents will remove most soils but will not remove watersoluble salts unless specially selected. Proprietary solutions designed to clean zinc surfaces are available. XI.2 New zinc-coated steel surfaces that cannot be treated in accordance with these methods prior to painting can be exposed to the weather for at least 6 months prior to painting to allow the surface to oxidize.5 N' XI.I--There are special primers that obviate the need for weathering--U.S. Fed. Spec. TT-P-641 and CGSB, l-GP-198 are examples. 5Literature on painting zinc-coated steel surfaces may be obtained from the American Zinc Institute, 292 Madison Ave., New York, NY 10017, or from th: National Paint, Varnish, and Lacquer Assoc., 15 Rhode Island Ave., N.W., Washington, DC 20005. ; X2. IDENTIFYING THE PRESENCE OF AND REMOVING CHROMATE TREATMENTS USED AS WET-STORAGE (ALSO CALLED HUMID-STORAGE) STAIN INHIBITORS X2.1 One of the inhibitors used by producers of zinccoated steel is a hexavalent chromium solution. This treat ment prevents Method D from working properly. X2.2 If zinc-coated steel to be painted is galvanized to order, the order should prohibit the use of hexavalent chromium humid-storage stain treatments. X2.3 Hexavalent chromium treatment can be removed from galvanized surfaces by one of the following three methods: X2.3.1 Weathering the surfaces for six months. X2.3.2 Abrading the surfaces by sanding. X2.3.3 Brush-off abrasive blast cleaning. X2.4 The presence of hexavalent chromium on gabsnized surfaces can be determined by spot testing with ' ? : 252 DUP05 02 97435  esin, the pplied by er coater. recoating ftened by The film otes good self. Two age matee-package uire daily ness within oiler, or dip Jnder the alvanized 2 metal to d make it rther im, B, C, or atment-- l the zinc netal ions O'C). The lorphous, increases treatment ion. 0 2092 diphenylcarbohydrazide solution. The spot test can also be used to evaluate the effectiveness of preparation to remove the treatment. X2.5 Make the spot test solution as follows: X2.5.1 Dissolve 0.5 g of 1,5-diphenylcarbohydrazide powder in a mixture of 20 mL acetone and 20 mL denatured ethanol. Heat the mixture in a warm water bath if necessary. X2.5.2 Dilute 20 mL of concentrated phosphoric acid to 40 mL by slowly adding to 20 mL of distilled or deionized water. X2.5.3 Add the dilute phosphoric acid to the acetonealcohol solution. X2.5.4 Store the solution away from light. Discard if it becomes discolored. Preferably make fresh solution as needed using proportionally smaller amounts of ingredients. X2.6 Conduct the spot test as follows: X2.6.1 Degrease the test spot on the galvanized surface. X2.6.2 Place several drops of the test solution on the galvanized surface. X2.6.3 If no color develops in the solution within 10 s, hexavalent chromium is not present. X2.6.4 If solution droplets turn a pink to purple color, then hexavalent chromium is present. X2.6.5 Conduct the spot test on several representative spots on each individual piece of galvanized steel. X2.6.6 Test every piece of galvanized steel that is to be treated for painting. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk o1 infringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technicsI committee and must be reviewed every five years and itnot revised, either reapproved or withdrawn. Your comments are levied either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to th ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. s prior to : need for P-198 are red from the , or from the Ave., N.W., GS ing three on galvating with 253 DUP0502 97436 Last ASTM Designation: D 2134 - 66 (Reapproved 1980)e1 Standard Test Method for Softening of Organic Coatings by Plastic Compositions This method covers the determination of the relative degree of surface softening of organic coating by plastic compositions under specified exposure conditions. Formerly under the jurisdiction of Committee D-20 on Plastics, this test method was discontinued in 1990. 9 De 1. Scope 1.1 Thes apparent v properties range from 1.2 This problems a user of th health prat limitations, 2. Referen 2.1 AS1 E 1 Sppi 3. Summa 3.1 Tes : viscosity c torque on material. 3.2 Tes shear thir propertie are deter [ tional-tyf diately p controllei 4. Signif | 4:1Te: j viscosity two or n I material i j 4.2 Wi 254 1 These u Paint andj.F j Subcommitt rials. j Current e ; published as | 2 Annual 3 pierce, and Resins v No. 557,19 DUP0502 97437 Designation: D 2196 - 86 (Reapproved 1991)e1 Standard Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield) Viscometer1 This standard is issued under the fixed designation D 2196; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies ofthe Department ofDefense to replace Method 42B7 ofFederal Test Method StandardMr. 141A. Consult the DoD IndexofSpecifications andStandardsforthe specific year ofissue which has been adopted by tke Department ofDefense. " N' --Section 24 was added editorially in August 1990. 1. Scope 1.1 These test methods cover the determination of the apparent viscosity and the shear thinning and thixotropic properties of non-Newtonian materials in the shear rate range from 0.1 to 50 s_1. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: E 1 Specification for ASTM Thermometers2 3. Summary of Test Methods 3.1 Test Method A consists of determining the apparent viscosity of coatings and related materials by measuring the torque on a spindle rotating at a constant speed in the material. 3.2 Test Methods B and C consist of determining the shear thinning and thixotropic (time-dependent) rheological properties of the materials.3 The viscosities of these materials are determined at a series of prescribed speeds of a rota tional-type viscometer. The agitation of the material imme diately preceding the viscosity measurements is carefully controlled. 4. Significance and Use 4.1 Test Method A is used for determining the apparent viscosity at a given rotational speed, although viscosities at two or more speeds better characterize a non-Newtonian material than does tke single viscosity measurement. 4.2 With Test Methods B and C, the extent of shear 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.24 on Physical Properties of Liquid Paints and Paint Mate rials. ... Current edition approved Aug. 29, 1986. Published October 1986. Originally Published as D 2196 - 63 T. Last previous edition D 2196 - 81. 2 Annual Book ofASTM Standards, Vol 14.03. 3 Pierce, P. E., "Measurement of Rheology of Thixotropic Organic Coatings and Resins with the Brookfield Viscometer," Journal ofPaint Technology, Vol 43, No. 557, 1971, pp. 35-43. thinning is indicated by the drop in viscosity with increasing viscometer speed. The degree of thixotropy is indicated by comparison of viscosities at increasing and decreasing vis cometer speeds (Test Method B), viscosity recovery (Test Method B), or viscosities before and after high shear (combi nation of Test Methods B and C). The high-shear treatment in Test Method C approximates shearing during paint appli cation. The viscosity behavior measured after high shear is indicative of the characteristics of the paint soon after application. 5. Apparatus 5.1 Rotational-type viscometers having at least four speeds, such as: 5.1.1 Brookfield Viscometer,* Model LVF, having four rotational speeds, or Model LVT having eight rotational speeds, with set of four spindles; or 5.1.2 Brookfield Viscometer, Model RVF, having four rotational speeds, or Model RYT having eight rotational speeds, with set of seven spindles. 5.2 Thermometer--ASTM thermometer having a range from 20 to 70'C and conforming to the requirements for Thermometer 49C as prescribed in Specification E 1. 5.3 Containers, round 1-pt (0.5-L) can, 33/s* in. (85 mm) in diameter, or 1-qt (1-L) can, 4 in. (100 mm) in diameter. 5.4 Shaker,s or equivalent machine capable of vigorously shaking the test specimen. 6. Materials 6.1 Standard Oils,6 calibrated in absolute viscosity, millipascal seconds. 7. Calibration of Apparatus 7.1 Select at least two standard oils of viscosities differing by at least 5 P (0.5 Pa-s) within the viscosity range of the material being measured and in the range of the viscometer. Condition the oils as closely as possible to 25.0C (or other 4 Brookfield viscometers are available from the Brookfield Engineering Labora tories, Inc., 240 Cushing St, Stoughton, MA 02072. 5 A reciprocating shaker may be obtained from the Red Devil Tools, 2400 Vauxhall Rd., Union, NJ 07083. 4 Absolute viscosity standards are available in 1-pt samples from The Cannon Instrument Co., P.O. Box 16, State College, PA 16801, or Brookfield Engineering Laboratories, Inc., 240 Cushing St., Stoughton, MA 02072. 255 DUP050297438 D 2196 agreed-upon temperature) for 1 h in a l-pf(0.5-L) can, 33/s in. (85 mm) in diameter. Measure the viscosities of each oil as described in Test Method B (Section 13) taking readings only at increasing speeds (13.7). Make certain that the spindle is centered in the container prior to taking measure ments. N' 1--The Brookfield LV and RV series viscometers are equipped with a spindle guard leg. The spindle/speed multiplying factors (Table 1) are designed for use with the guard leg in place except for the following conditions: RV series when the factors are the same with or without the guard leg for spindles No. 3 through 7; or LV series when the factors are the same with or without the guard leg for spindles No. 3 and 4. 7.1.1 Calibration in a 1-pt (0.5-L) can is always possible with the LV series viscometer with the guard leg attached. Calibration of the RV series viscometer in the 1-pt can must be done with spindles No. 3 through 7 without the guard leg. If the No. 1 or No. 2 spindles are to be used, calibration is carried out in the 1-qt (1-L) can with the guard leg attached. 7.2 Combining the tolerance of the viscometer (1 %, equal to the spindle/speed factor) and the tolerance of the temperature control (typically 0.5C at 25I>C) it is reason able to assume that a viscometer is calibrated if the calcu lated viscosities are within 5 % of the stated values (see Table 2 for examples of the considerable change in viscosity with temperature exhibited by standard oils). If measure ments are not made at 25C, then the stated viscosities should be corrected to the temperature at which they are measured. If the viscosities determined in 7.1 differ from the stated values of the viscosity standard by more than 5 %, calculate new factors for each spindle/speed combination as follows: /= V/s (1) where: f = new factor for converting scale reading to viscosity, cP (mPa-s), V = viscosity of standard oil, mPa-s, and s = scale reading of the viscometer. TABLE 1 Factors for Converting Brookfield Dial Readings to Centipoises (Millipascal Seconds) N' --M = 1000. Speed, rpm RV Series Factors Spindles 12 3 4 5 6 7 0.5 1 2 2.5 4 5 10 20 50 100 200 800 2000 4000 8000 20M 100 400 1000 2000 4000 10M 50 200 500 1000 2000 5M 40 160 400 800 1600 4M 25 100 250 500 1000 2.5M' 20 80 200 400 300 2M 10 40 100 200 ' 400 INI 5 20 50 100 200 500 2 8 20 40 80 200 t 4 10 20- 40 100' 60M 40M 20M 16M 10M 8M 4M 2M 800 400 LV Series Factors Spindles 123 4 0.3 0.6 1.5 3.0 6 12 30 80 200 1000 4000 20M 100 500 2000 10M 40 200 800 4M 20 100 400 2M 10 50 200 1M 5 25 100 -- 500 . 2 10 40 200 1 5 20 100 7.3 Prepare a table of new factors similar to that furnished with the viscometer (Table 1) for the spindle/speed combina tions worked out in 7.2. Spindle/speed factors vary inversely with speed. 8. Preparation of Specimen 8.1 Fill a 1-pt or 1-qt can with sample to within 1 in. (25 mm) of the top with the sample and bring it as close as possible to a temperature of 25C or other agreed-upon temperature prior to test. 8.2 Vigorously shake the specimen on the shaker or equivalent for 10 min, remove it from the shaker, and allow it to stand undisturbed for 60 min at 25C prior to testing (Note 2). Start the test no later than 65 min after removing the can from the shaker. Do not transfer the specimen from the container in which it was shaken. N' 2--Shake time may be reduced if necessary, or as agreed upon between the purchaser and manufacturer, but, in any case, should not be less than 3 min. ofi vii Or str of be so If fc w V f s TEST METHOD A--APPARENT VISCOSITY 9. Procedure 9.1 Make all measurements as close as possible to 25C, or other agreed-upon temperature. 9.2 Place the instrument on the adjustable stand. Lower j the viscometer to a level that will immerse the spindle to the proper depth. Level the instrument using the attached spirit I level. 9.3 Tilt the selected spindle (Note 3), insert it into one 1 side of the center of the surface of the material, and attach the spindle to the instrument as follows: Firmly hold the | upper shaft coupling with thumb and forefinger; screw left-hand thread spindle coupling securely to the upper shaft coupling being very careful when connecting to avoid undue | side pressure which might affect alignment. Avoid rotating the dial so that pointer touches the stops at either extreme of the scale. j N' 3--Select the spindle/speed combination that will give a minimum scaie reading of 10 but preferably in the middle or upper portion of the scale. The speed and spindle to be used may differ from this by agreement between user and producer. 9.4 Lower the viscometer until the groove (immersion mark) on the shaft just touches the material. Adjust the viscometer level if necessary. Move the container slowly in a horizontal plane until the spindle is located in approximately the center of the container so that the test will be run in a, region undisturbed by the lowering of the spindle. . 9.5 Turn on the viscometer. Adjust the viscometer to th^ j rpm. selected (Note 3) for the material under test. Allow the viscometer to run until the pointer has stabilized (Note 4). After the pointer has stabilized, depress the clutch and switch s 1 t , TABLE 2 Viscosity Variation of Cannon Viscosity Standards About the 25C Temperature Point Cannon Viscosity Standard S-600 S-2000 s-eooo Viscosity at 25C, cP (mPa-s) t 400 4 900 20 000 Viscosity Change With +1C at 25C, oP (mPa-s) 87.7(6.26%) 332 (6.77 %) 1462.3 (7.31 %) 256 DUP05 02 97439 i 1 in. (2s s close as reed-upon shaker or and allow to testing removing nen from greed upon ould not be > 25'C, or d. Lower lie to the ted spirit into one id attach hold the r, screw per shaft id undue rotating treme of ill give a or upper iffer from mersion just the wly in a ornately un in a :r to the llow the Vote 4). d switch dards -i +ic s) 1 D 2196 the motor so that when it stops, the pointer will be in (Note 5). N' 4--In thixotropic paints, the pointer does not always stabilize. 0,, occasion it reaches a peak and then gradually declines as the stnJcture is broken down. In these cases, the time of rotation or number 0f revolutions prior to reading the viscometer should be agreed to 'tween user and manufacturer. N' 5--Always release the dutch while the spindle is still immersed jo that the pointer will float, rather than snap back to zero. jO. Calculation 10.1 Calculate the apparent viscosity at each speed, as follows: V = fs where: y s viscosity of sample in centipoises, mPa-s, r = scale factor furnished with instrument (see Table 1), and s = scale reading of viscometer. 11. Report 11.1 Report the following information: 11.1.1 The Brookfield viscometer model and spindle, 11.1.2 The viscosity at the spindle/speed utilized, 11.1.3 The specimen temperature in degrees Celsius, and 11.1.4 The shake time and' rest period, if other than specified. 12. Precision and Bias 12.1 Precision--See Section 23 for precision, including that for measurement at a single speed. 12.2 Bias--No statement of bias is possible with this test method. ' 9 ' ' " ' --P< ( < "' ( ' { < { !' ' " CONDITIONS, DEGREE OF SHEAR THINNING AND THIXOTROPY 13. Procedure 13.1 Make all measurements with the Brookfield viscometer as close as possible to 2SC, or other agreed upon temperature. 13.2 Adjust the instrument and attach the spindle as in 9.2 through 9.4. 13.3 Set the viscometer at the slowest rotational speed (Notes 5 and 6). Start the viscometer and record the scale reading after ten revolutions (or other agreed-upon number of revolutions). N"#' 6--When the eight speed viscometers (RVT and LVT) are used, lower or higher speeds than that permitted by the four speed viscometers may be used upon agreement between producer and user. 13.4 Increase the viscometer speed stepwise and record the scale reading after ten revolutions (or equivalent time for each spindle/speed combination) at each speed After an ob servation has been made at the top speed, decrease the speed in steps to the slowest speed, recording the scale reading after ten revolutions (or equivalent time) at each speed. N$%' 7--It is preferable to change speed when the motor is running. 13.5 After the last reading has been taken at the slowest speed, shut off the viscometer and allow it and the specimen to stand undisturbed for an agreed-upon rest period. At the end of the rest period, start the viscometer at the slowest speed and record the scale reading after ten revolutions (or other agreed-upon number of revolutions). 14. Calculations and Interpretation of Results 14.1 Calculate the apparent viscosity at each speed as shown in Section 9. 14.2 If desired, determine the degree of shear thinning by the following method: 14.2.1 Shear Thinning Index (sometimes erroneously called the thixotropic index)--Divide the apparent viscosity at a low rotational speed by the viscosity at a speed ten times higher. Typical speed combinations are 2 and 20 rpm, 5 and 50 rpm, 6 and 60 rpm but selection is subject to agreement between producer and user. The resultant viscosity ratio is an index of the degree of shear thinning over that range of rotational speed with higher ratios indicating greater shear thinning. 14.2.2 A regular or log-log plot of viscosity versus viscometer speed in rpm may also be useful in characterizing the shear-thinning behavior of the material. Such plots may be used for making comparisons between paints or other materials. 14.3 If desired, estimate the degree of thixotropy (under conditions of limited shearing-out of structure) by one of the following methods: 14.3.1 Calculate the ratio of the slowest speed viscosity taken with increasing speed to that with decreasing speed. The higher the ratio, the greater the thixotropy. 14.3.2 Calculate the ratio of the slowest speed viscosity taken after the rest period to that before the rest period. The higher the ratio, the greater the thixotropy. 15. Report 15.1 Report the following information: 15.1.1 The Brookfield viscometer and spindle, 15.1.2 The viscosities at increasing and decreasing spindle speeds, 15.1.3 The rest period time and the viscosity at the end of that time, 15.1.4 The specimen temperature in degrees Celsius, and 15.1.5 The shake time if other than that specified. 15.2 Optional Reporting: 15.2.1 Degree of Shear Thinning--Shear thinning index and speeds over which it was measured (14.2). 15.2.2 Estimated Degree, of Thixotropy (under conditions of shearing-out of structure)--Ratio of the lowest speed viscosities, for both increasing and decreasing speeds; or ratio ofthe lowest speed viscosities before and after the rest period, and speed at which they were measured (14.3). 16. Precision and Bias 16.1 Precision--See Section 23 for precision, including that for measurement of the shear thinning index (ratio of viscosity at 5 r/min to that at 50 r/min). It has not been possible to devise a method for determining precision for viscosities at increasing and decreasing speeds other than as individual measurements. No attempt was made to deter mine the precision of the measurement of the degree of thixotropy because this parameter is dependent on the material, the time of the test, and other variables. 257 DUPO 50297440 # D 2196 16.2 Bias--No statement of bias is possible-with this test method. TEST METHOD C--VISCOSITY AND SHEAR THINNING OF A SHEARED MATERIAL 17. Apparatus 17.1 High-speed laboratory stirrer with speeds of at least 2000 rpm and equipped with a 2-in. (50-mm) diameter circular dispersion blade.7 18. Preparation of Specimen 21.1.1 The Brookfield viscometer model and spindle, 21.1.2 The viscosities at decreasing spindle speeds, 21.1.3 The specimen temperature in degrees Celsius, and 21.1.4 The speed of the high-speed mixer, size of blade, and time of mixing if different from method. 21.2 Optional Reporting: 21.2.1 Degree of Shear Thinning-Shear thinning index and speed over which it was measured (14.2). 21.2.2 Estimated Thixotropy--Ratio of lowest speed vis cosities before and after shear and the speed at which they were measured. 18.1 Insert the 2-in. (50-mm) blade into the center of the can (4.3) so that the blade is about 1 in. (25 mm) from the bottom. Run the mixer at 2000 rpm (Note 8) for I min. NOTE 8--Materials may be sheared at other speeds using other size blades upon agreement between producer and user. 19. Procedure 19.1 Immediately insert the same spindle used in Test Method B into the sheared material in the same manner as in 22. Precision and Bias 22.1 Precision--The precision for individual viscosity measurements is the same as for Test Method A in Section 23. No attempt has been made to determine the precision of the shear thinning index or degree of thixotropy for Test Method C for the reasons given in 16,1. 22.2 Bias--No. statement of bias is possible with this test method. 1. Scopi 1.1 T adhesior lacquer 1.2 T safety p Section 9. 23. Summary of Precision 19.2 Start the viscometer and adjust to the highest speed used in Test Method B (13.5). Record the scale reading after 23.1 In an interlaboratory study of Test Methods A and B, ten revolutions (or other agreed-upon number of revolu eight operators in six laboratories measured on two days the tions). 19.3 Decrease the viscometer speed (Note 7) step-wise and viscosities of four architectural paints'comprising a latex flat, a latex semi-gloss, a water-reducible gloss enamel, and an if record the scale readings at each speed down to the lowest speed used in Test Method B, recording the scale reading alkyd semi-gloss, that covered a reasonable range in viscosi ties and were shear thinning. Measurements at increasing ! after ten revolutions at each speed (or other agreed-upon speeds of 5, 10, 20, and 50 r/min (equivalent to eight number of revolutions). operators testing 16 samples) were used to obtain the precision of Test Method A. The within-laboiatory coeffi responsi priate sc bility of 2. Refer 2.1 A D 609 Pair D823 Thi. 20. Calculations and Interpretation of Results 20.1 As in Test Method B, calculate the viscosities at each decreasing speed. 20.2 If desired, calculate the degree of shear thinning by the method given in Test Method B, 14.2. The measured viscosity behavior after shearing is essentially that of the paint immediately after application (disregarding changes in solids). 20.3 If desipd, estimate the degree of thixotropy (under conditions of complete shearing-out of structure) by calcu lating the ratio of the lowest speed viscosities before and after shear. The lowest speed before-shear viscosity is taken from Test Method B, 14.1, at the lowest increasing speed. The lowest speed after-shear viscosity is taken from 20.1. The higher the ratio, the greater the thixotropy. cient of variation for Test Method A (angle speed) was found to be 2.49 % with 121 degrees of freedom and for Test Method B (Shear Thinning Index) 3.3 % with ,31 degrees of freedom. The corresponding between-Iabpratories coeffi cients are 7.68 % with 105 degrees of freedom and 7.63 % with 27 degrees of freedom. Based on these coefficients the following criteria should be used forjudging the acceptability of results at thei95 % confidence level: 23.1.1 Repeatability--Two results obtained by the same operator at different times should be considered suspect if they differ by more than 7 % relative. for single speed viscosity and 9.5 % relative for shear thinning index. 23.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than 21.6 and 22.1 % relative, respec tively, for the same two test methods. Tes D 100 Thi D 118 Dry to a D 14(3 Dp plie 3. Sum) 3.1 T thicknes surface pushing loaded i 21. Report 21.1 Report the following information: 24. Keywords 24.1 Brookfield' viscometer, non-Newtonian; rheologieal from the 4. Signi properties; rheology;, rotational;, shear thjnuing; thixotropic; 4.1 G 7 Cowles or Shar type mixer/disperser. thixotropy; viscometer, viscosity , substrate been fou The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection, coatings with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility'. ^ I~ This standard is subject to revision at any time by the responsible technical committee and'must be reviewed erery five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful-consideration af a meeting of thd responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldjnake your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19.103. ., 1 This te and Relate | mittee D01 258 DUP050297441 I Designation: D 2197 - 86 (Reapproved f99f)'' and 'lade,, ndex 1 visthey 'OSlty ction on of Test s test nd B, sthe i flat, d an scosiasing eight t the oeffibund Test :es of oefFi63% :s the bility same ct if seed tera ct if .pec- ugical ropic; Standard Test Method for Adhesion of Organic Coatings by Scrape Adhesion1 This standard is issued under the fixed designation D 2197; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last,revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (<) indicates an editorial change sinoe the last revision or reapprovai. This method has been approvedfor use by agertices of the Department of Defense to replace Method 6303 of Federal Test Metkod Standard No. 141C andfor listing in the DoD Index ofSpecifications and Standards. ei N&'' --Keywords were added editorially in July 1991, '' 1. Scope 1.1 This test method covers the determination of the adhesion of organic coatings such as paint, varnish, and lacquer when applied to smooth, flat (planar) panel surfaces. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the _ responsibility ofthe user of this standard to establish appro-"' priate safety and health practices and determine the applica bility of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry-Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings AP" plied to a Nonferrous Metal Base2 3. Summary of Test Method 3.1 The materials under test are applied at uniform thickness to flat panels, usually sheet metal of uniform surface texture. After drying, the adhesion is determined by pushing the panels beneath a rounded stylus or loop that is loaded in increasing amounts until the coating is removed from the substrate surface. ratings for a series of coated panels exhibiting significant differences in adhesion. 5. Apparatus 5.1 Application Equipment, as described in Test Methods D 823. 5.2 Film-Thickness Measuring Apparatus, as described in Test Methods D 1005, D 1186, or D 1400. 5.3 Balanced-Beam, Scrape-Adhesion Tester (Fig. I),3 consisting ofa balanced beam to which is secured a platform for supporting weights, and a rod at an angle of 45 that holds the scraping loop. The rod shall be set so that the scraping loop contacts test surfaces directly below the weights. The loop shall be Vis-in. (1.6-mm) diameter rod, bent into a "U" shape with an outside radius of 0.128 0.002 in. (3.25 0.05 mm) and hardened to Rockwell HRC 56 to 58, and shall be chromium plated and polished. 6. Preparation of Specimens 6.1 Apply the materials under test to panels of the composition and surface condition on which it is desired to determine adhesion. The panel material (6.1.IX surface preparation, thickness, and number of coats shall be speci fied or agreed upon by the seller and the purchaser. Apply uniform coatings and air dry or bake under conditions of humidity and temperature mutually agreeable to the seller and purchaser. Either mask the panel or remove material after, application, so that xh in. (13 mm) at one end of the panel is uncoated. ,6.1.1 The surface of the panel must be hard enough that it will not be damaged by the scraping loop. If no panel material is specified, use 0.03Z-in. (0.8-mm) cold-rolled carbon steel prepared in accordance with Methods B or C of Methods D 609. 4. Significance and Use 4.1 Coatings to perform satisfactorily must adhere to the substrates on which they are applied. This test method has been found useful in differentiating the degree ofadhesion of coatings to substrates. It is most useful in providing relative 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint ad Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.23 on Physical Properties of Applied Paint Films. Current edition approved Aug. 29, 1986. Published October 1986. Originally Published as D 2197 - 63 T. Last previous edition D 2197 - 85. 2 Annual Book ofASTM Standards, Vol 06.01. 7. Conditioning and Number of Tests 7.1 Condition the test panels for at least 48 h at 73.5 3,5F (23 2C) and 50 5 % relative humidity, and test in the same environment,' or immediately on removal there from, unless otherwise specified or agreed by the seller and the purchaser. Test at least two replicate specimens of each material. 3 The tester is available from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. Other apparatus of demonstrated equivalency may be used. 259 DU P050297442 D 2197 . ::*?! FIG. 1 Balanced-Beam Scrape-Adhesion Tester 8. Procedure 8.1 When using the instrument shown in Fig. 1, level the base plate of the apparatus and place it so that the weight holder is toward the operator. This places the beam release on the operator's right and allows freedom to move the test specimen manually under the weighted scraping element (loop). Adjust the main bearing support so that the beam is _ balanced in the horizontal plane when the loop is just"' touching the specimen surface. 8.2 Raise the beam and lock it. Wipe the loop with clean cloth or chamois. Place a test panel on the sliding platform so that it may be moved away from the operator and the uncoated portion is toward the main beam support. Place weights on the weight support using an initial amount that is estimated to be appropriate for the particular coating. Carefully lower the beam until the loop rests on the uncoated portion ofthe test specimen and the hill load is applied, then slowly (1 to 2 s/in.) push the sliding platform away from the operator for a distance of at least 3 in. (75 mm). If the coating is removed, continue the testing, using successively smaller loads (0.5-kg increments) until the coating is not removed. If the coating is not removed by the initial scrape, continue the testing, using successively larger loads (0.5-kg increments) until the coating is removed or until the maximum load of 10 kg has been applied. Use a new area of the test surface each time a scrape is made. 8.3 When the critical load has been approximately lo cated, repeat the test five times at each of three loadings: above, below, and at the load determined in the first trial. Apply the different loads in random fashion so that all scrapes at one load are not made in succession or on one panel. 8.3.1 Periodically examine the loop to ensure that the original smooth surface is intact. If the contacting surface is worn, reverse the loop. When both sides are worn, replace with a new loop. 8.4 For each applied load, tabulate the number of times the coating was removed or adhered. The load where the scrape results change from mainly adhering to mainly removed, ignoring the first Vi in. (13 mm) of the scratch if the coating was removed, is the adhesion failure end point. 9. Report 9.1 Report the following information: 9.1.1 Load in kilograms at the adhesion failure end point 9.1.2 Panel material and surface preparation. 9.1.3 Dry-film thickness. 9.1.4 Any deviation from the specified procedure. [; [ | ; 10. Precision 10.1 Correlation--This method was developed when cor relation with other methods of assessing adhesion was considered to be of equal importance to the agreement between results obtained in the same or different laboratories. It was established that when materials differing widely in hardness and adhesion were evaluated by a number of experienced personnel in several laboratories, the adhesion results obtained using this method correlated well with those obtained with several other methods. 10.2 Precision--If sufficient cooperators can be obtained, an interlaboratory study will be conducted to establish precision. | ; j \ 11. Keywords | 11.1 adhesion, scrape; balanced-beam scrape adhesion I tester '' S 1. of file i obi In mai I atu adi tke m m' 2. 2 / A E E 2 F F E F 2 h The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ot any such patent rights, and the risk ot infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and musl be reviewed every rive years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standardor for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments havenot received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 3. f 13 pan dry and I mitte Cu Publi: 260 DUP050297443 Designation: D 2198 - 84 (Reapproved 1989)c1 face is splace times re the aainly itch if >oint. point. ncort was ;ment oratoiely in >er of lesion those ined, blish ssion Standard Test Method for Stain Removal From Multicolor Lacquers1 This standard is issued under the fixed designation D 2198; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. tl N()' --Editorial changes were made throughout in April 1989. t. Scope 1.1 This test method covers a procedure for the removal of pencil, crayon, and grease stains from multicolor lacquer films that have been applied to primed steel panels. N*+' --Due to the nature of the test, comparable results can be obtained only when exactly the same materials and apparatus are used. In this test method it has not been found possible to describe the materials and apparatus adequately in more than general terms. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1. Referenced Documents 2.1 ASTM Standards: A 109 Specification for Steel, Strip, Carbon, Cold-Rolled2 A 366/A 366M Specification for Steel, Sheet, Carbon, Cold-Rolled, Commercial Quality2 D 209 Specification for Lampblack Pigment3 D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products4 2.2 U. S. Federal Specifications.s Fed. Spec. EE-0-451C Specification for Oleo (Margarine) Fed. Spec. TTV-121C Specification for Varnish, Spar, Water Resisting Fed. Spec. VV-O-55! Specification for Oil, Lubricating, Marine and Engine, Mineral Fed. Spec. VV-P-236 Specification for Petrolatum 2.3 U. S. Military Specification.J MIL-P-11414A Specification for Primer Coating, Lacquer, Rust Inhibiting 3. Summary of Test Method 3.1 Three 6V2 by 17-in. (165 by 430 mm) primed steel panels are sprayed with multicolor lacquer and allowed to dry for 24 h. Varnish is then applied to the ends of the panels ' This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Aug. 31, 1984. Published January 1985, Originally published as D 2198 - 63 T. Last previous edition D 2198 - 68 (1979)e|. * Annual Book cfASTM Standards, Voi 0 i .03. 3 Annual Book cfASTM Standards, Voi 06,02. 4 Annual Book ofASTM Standards, V0IO6.OI........ 1 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. and allowed to dry 72 h. The three stains are applied by a mechanical apparatus and removed by washing. 4. Significance and Use 4.1 The procedure described in this test method is in tended as an aid in evaluating the ease of removal for surface stains encountered by surfaces coated with multicolor lac quers. 5. Apparatus and Materials 5.1 Steel Panels, 6V2 by 17 in. (165 by 430 mm), 20-gage cold-rolled steel conforming to Specification A 109 or Spec ification A 366. 5.2 Washability Machine.6 5.3 Lacquer Primer, conforming to MIL-P-11414A. 5.4 Drafting Pencil. 5.5 China Marking Crayon. 5.6 Wetting Agent.7 5.7 Amorphous Silica. 5.8 Diaper Cloth. 5.9 Varnish, clear and waterproof, conforming to Fed. Spec. TT-V-121C or equal cut in mineral spirits. 5.10 Carriage, for mounting pencil and crayon. 5.11 Arm, extendible, for mounting mohair roller. 5.12 Mohair Roller, VA in. (40 mm), for application of grease stain. 5.13 Glass Plate, 4 by 7 in. (100 by 175 mm), for holding grease stain. 5.14 Grease--The grease shall consist of the following ingredients: 5.14.1 Lanolin, anhydrous, 50 g, 5.14.2 Petrolatum, 50 g, conforming to Fed. Spec. VVP-236, 5.14.3 Margarine, 30 g, conforming to Fed. Spec. EE0-451C, 5.14.4 Mineral Oil, 10 g, conforming to Fed. Spec. W-0-551, and 5.14.5 Lampblack, 5 g, conforming to Specification D209. 6. Preparation of Panels 6.1 Prepare three 6V2 by 17-in (165 by 430-mm) steel panels in accordance with Methods D 609. Spray a 0.5-mil 6 Gardner Model AG810O, available from Byk-Gardner, Inc., Gardner Labora tory, 2433 Linden Ln., Silver Spring, MD 20910, has been found suitable for this purpose. 7 Triton X-100, available from Rohm and Haas Marketing Services, Independ ence Mall West, Philadelphia, PA 19105, has been found suitable for this purpose. 261 1 DUP050297444 * tr l D2198 (13-fim) film of the lacquer primer and air dry for 24 h at amount of grease on the roller. normal room temperature. With the primer reduced 100 % 7.2 Removal ofStains: with the recommended thinner, one wet coat will give 7.2.1 Cut the diaper doth into a strip 5% by 63A in. (150 approximately 0.5 mil. by 170 mm) and fold to three thicknesses to give 2 by 6% in. 6.2 Spray two coats of multicolor lacquer over the primer (50 by 17(5 mm), keeping the embossed side out and the raw with the atomization pressure adjusted to get complete edges in. Soak the folded cloth in water, squeeze out the covering and allow 1 h between coats for flash off. excess water, and place on the 2-lb (900-g) abrasion boat 6.3 To protect the end of the panels in handling and (load boat with weight if necessary). Place 2 g of No. 22 silica scrubbing, brush one coat of varnish on the 5 in. (125 mm) wet with 2 mL ofa 5 % wetting agent solution and smear this of the end of each panel after 24 h of drying of the paste uniformly on the scrubbing area of the cloth with a multicolor. Leave 7 in. (175 mm) of exposed test lacquer in spatula. the center of the panels and allow the varnish to dry 72 h 7.2.2 Start the scrubbing test using the Gardner Wash- before staining the panels. Test within 1 to 2 h after staining. ability Machine and record the number of cycles required to remove completely each ofthe three stains. Ifany of the stain 7. Procedure is'not removed after 100 cycles, add 1 mL of 5 % wetting agent'solution to rewet the cloth and continue the test. 7.1 Application ofStains: Repeat at 100-cycle intervals stopping after 500 cycles. Rinse 7.1.1 Pencil and China Marking Crayon--Make both the the panel in running water and allow to dry. pencil lead and the crayon flat by rubbing over fine sandpaper before application of pencil and crayon stains. 8. Report Mount the pencil vertically in the carriage so that it rests Ji.l Record the results as the number of cycles (double with its own weight on the surface to be stained. Add an strokes)' needed to remove each stain completely. Describe additional weight so that the total is 40 g. Move the pencil any stain that is not removed after 500 cycles as the percent over the panel 5 strokes perpendicular to the abrasion boat of stain remaining on each of three panels and record the piath. Repeat this procedure with the crayon. Stain three mean of the three panels. panels. 7.1.2 Grease Stain--Apply 1 g of grease to a 4 by 7-in ` 9. Precision -A. ' f (100 by 175-mm) glass plate and smooth with a rubber roller. 9.1 Because of the variations that can arise from the | Pass a lVi-in. (40-mm) mohair roller mounted on the application of the stains, meaningful estimates of precision f extendible arm over the greased plate making three stripes cannot be given. In round robin tests fairly good agreement ! and removing the grease down to the glass on each stripe so was obtained by the cooperators when the method of :; that the entire surface ofthe roller is uniformly coated. Then application of stains was the same. ; I pass the. roller over the panels coated with the lacquer under I test. Make one stripe on the glass panel between the staining 10. Keywords 1; of each subsequent panel under test to maintain a uniform 10.1 stain removal; multicolor lacquers; lacquer The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such ;! patent rights, and the risk of Infringement of such rights, are entirely their bwn responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either foprevision of this standard or lor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Commlttee.on Standards, 1916 Race St., Philadelphia, PA 19103. <1 I 1. Scope 1.1 Tb surement fabric to contact. N,-' -- reliable res coated. 1.2 Tl ations, a address t the respt approprit applicaht 2. Sumi 2.1 A tioned cc assembly temperat for man print at test time 3. Signil 3.1 PI to coatir place, i method tendenc 4. App j 4.1 D `j > vide a j ; thicknes I double s \ 4.4 Sj I in. (6.3 i ! 4.5 H i of 2 ib c | 1 This ti Related Cc j 001.55 Fai [ Current - published i 262 DUP050297445 Designation: D 2199 - 82 (Reapproved 1987) in.(150 y 6% in. the raw out the on boat 22 silica near this i with a r Washluired to the stain wetting the test, is. Rinse (double Describe percent :ord the om the irecision reement thod of Standard Method for Measurement of Plasticizer Migration From Vinyl Fabrics to Lacquers1 This standard is issued under the fixed designation D 2199; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. j. Scope 1.1 This method covers an accelerated test for the mea surement of a tendency for plasticizers in finished vinyl fabric to be transferred to coatings with which they come in contact. NOTE--Age offabric sample may affect results oftest. To ensure most pliable results, test with fabric sample closest in age to what will be toated. 1.2 This standard may involve hazardous materials, oper ations, and eqidpment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Summary of Method 2.1 A small sample of vinyl fabric is placed on a condi tioned coating film under a pressure of Vz psi (3.45 kPa). The assembly is placed in an oven for 3 days at elevated temperature. At the end ofthat time, the coating is examined for marring or softening. For coatings that may block or print at 50C or lower, a lower test temperature and a longer test time may have to be used. 3. Significance and Use 3.1 Plasticizers in finished vinyl fabric can be transferred to coatings with which they come in contact. When this takes place, objectionable marring and softening occur. This method covers an accelerated test for measurement of this tendency. 4. Apparatus 4.1 Drawdown Blade, 5-mils (125-pm) clearance to pro vide a wet film of approximately 2.5 mils (63 |xm) in thickness. 4.2 Plate Glass Panels. 4.3 Window Glass, 2 by 2-in. (51 by 51-mm) square, double strength. 4.4 Sponge Rubber, 2 by 2-in. (51 by 51-mm) square by `A in. (6.3 mm) thick. 4.5 Weights, flat-bottom, sufficient to place a total weight of 2 lb (910 g) on each test sample. 1This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee >01.55 Factory-Applied Coatings on Preformed Products. ................ Current edition approved OcL 29, 1982. Published January 1983. Originally Published as D 2199 - 63 T. Last previous edition D 2199 - 78. 4.6 Forced-Convection Oven, thermostatically controlled to 2C. 4.7 Photograph Roller? 4.8 Aluminum Foil. 5. Procedure 5.1 Apply the coating to the glass panel with the drawdown blade to provide a uniform film with an area of at least a 2-in. (51-mm) square and a dry thickness of at least 1 mil (25 pm) or as agreed upon. Dry the coating in accord ance with the recommendations of the manufacturer or for a minimum of 24 h at room temperature and 2 h at 50"C. 5.2 Preheat the glass plate bearing the coating, the 2 by 2-in. glass square, and the weights for 30 min at 50C. Place the square of vinyl fabric on the coating with care and ensure intimate contact by rolling with the photographic roller. Cover the fabric with foil, sponge rubber, glass, and weight in that order. The total weight shall be 2 lb (910 g). 5.3 Place the assembly in the forced convection oven at a temperature of 50C for 72 h. After removal from the oven and cooling, remove the weight, sponge rubber, and alu minum foil, and carefully remove the vinyl fabric. Note and report any resistance to removal. Wipe the surface of the fabric with a soft rag dampened with heptane and examine for removal of exuded plasticizer. 6. Rating 6.1 Rate the degree of migration by viewing the surface of the coating at a low angle against the light within 2 h after termination of heating and within 15 min of removal of the fabric. 7. Report 7.1 Report marring or softening, or both, on the scale of no change, faint imprint, severe imprint, or marring. 7.2 If plasticizer is evident when the surface is wiped, this shall be reported. 8. Precision 8.1 This method does not result in a numerical value for precision but repeated tests have demonstrated that several laboratories will assign the same rating to various coating fabric combinations. Also, replicate tests by one laboratory are in good agreement. 2 A squeegee-type roller is satisfactory. 263 DU PO 50297446 # D 2199 The American Society for Testing and Materials takas no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users of fft/s standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is sublect to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments wkl receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hewing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. 1. Scot 1.1 1 series o differen designa Method depictic tion of cleaninj specific: be used Thee differen surface grades,. 100% r appeara method: thoroug 2. Refei 2.1 A Pic Sur 3. Tern 3.1 L 3.1.1 surface pictorial definitic cation.3 264 1 This st Related Co DO 1.46 on The pict and have b (Vis 1), anc Current published a 2 The pi quarters (r> Council, 4 seringskom JThe V available f Pittsburgh, DU P0502 97447 Designation; D 2200 - 91 Swedish Standards Association Standard SIS 05 59 00 Steei Structures Painting Council SSPC-Vis 1 Danish Standards Association Danish Standard DS 2019 European Committee of Paint and Printing ink Manufacturers' Association Standard Pictorial Surface Preparation Standards for Painting Steei Surfaces1 This standard is issued under the fixed designation D 2200; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval A superscript epsilon (i) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 The visual surface preparation standards consist of a series of color prints available as separate publications. Two different sets of photographs are described in this standard, designated as Method A (ISO/Swedish Standard2) and Method B (SSPC Standard3). The two methods differ iruthe depiction of the initial surface, in the definition and depic tion of the cleaning conditions, and in the number of cleaning methods included. Because of these differences, the specifier should state whether Method A or Method B should be used. The colored visual surface preparation standards represent different conditions of hot rolled steel before and after surface preparation. Prior to cleaning, there are four rust grades, A to D, that cover the range from intact mill scale to 100 % rusted and pitted steel. The standards then depict the appearance of the four grades after cleaning by one or more methods (for example, blast cleaning) to various degrees of thoroughness. 2. Referenced Documents 2.1 Adjuncts: Pictorial Surface Preparation Standards2 Surface Cleanliness Definitions3 3. Terminology 3.1 Definitions: 3.1.1 The cleanliness definitions for the Method A visual surface preparation standard appear in the text of the pictorial surface preparation standards publication.2 The definitions for Method B are found in a separate publi cation.3 1 This standard is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee 00] .46 on Industrial Protective Coatings. The pictorial standards described were prepared by the Swedish Corrosion Inst, and have been jointly approved by ASTM, the Steel Structures Painting Council (Vis 1), and the Swedish Standardizing Commission. Current edition approved Sept 15, 1991. Published November 1991. Originally published as D 2200 - 66. Last previous edition D 2200 - 85 {1989). 2 The pictorial surface preparation standards are available from ASTM Head quarters (request Adjunct No. 12-422000-00); the Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, PA 15213; and Sveriges Standardiseringskommission. Box 3295, Stockholm 3, Sweden. 3 The Visual Standards Method B and surface cleanliness definitions axe available from the Steel Structures Painting Council, 4400 Fifth Avenue, Pittsburgh, PA 15213. 4. Significance and Use 4.1 The appearance of the various degrees of blast cleaning are influenced by the initial rust grades of the steel being cleaned. The standards aid visually in judging and evaluating the degree of rusting before cleaning and the degree of cleaning of steel surfaces prior to painting. 4.2 Two methods for visual standards have evolved be cause of differences in the practice of using visual standards throughout the world. In Europe, the visual standards (Method A) are used as the primary means of determining the degree of cleaning. In the US, the SSPC written defini tions take precedence with the visual standards used as a supplement. The visual standards of Method B comply with the SSPC definitions. 5. Procedure and Interpretation Method A--ISO/Swedish Standard 5.1 Determine the method of cleaning to be used (for example, hand/power tool cleaning, abrasive blast cleaning, or flame cleaning). 5.2 Determine the initial condition of the steel in accor dance with four initial grades (A, B, C, or D). 5.3 Following the cleaning operation, compare the surface prepared with the photographs showing the degree of thor oughness for that particular initial condition. Select the degree that most closely corresponds to the prepared surface. 5.4 Repeat the procedure for representative areas of structure and record all three items (initial condition, method of cleaning, and degree of thoroughness achieved). Method B, SSPC Visual Standard 5.5 Determine the degree of blast cleaning to be em ployed. 5.6 Determine the initial condition of steel in accordance with photographs A, B, C, and D. 5.7 Following the cleaning operation, compare the pre pared surface with the photographs showing the degree of thoroughness for that particular initial condition. Select the degree that most closely corresponds to the prepared surface. 5.8 Repeat for all representative areas of structure and record for each area the initial condition and degree of thoroughness achieved. 5.9 When abrasives other than silica sand are used for 265 DU P050297448 # D 2200 blast dp!)niriS] consult the photographs in the appendix of the SSPC Standard for possible variations in appearance created by the abrasive type. N./' 1--Different steel surfaces show differences in shade, color, tone, pitting, flaking, mill scale, etc. To some extent, these differences between the actual steel surface and the visual standard can be reconciled between the painting contractor and the inspector. 6. Keywords 6.1 blast cleaning; flame cleaning; photographic standards for surface preparation; power tool cleaning; surface prepa ration; surface preparation standards The American Society for Testing and Materials takes no position respecting the validity of any patehtrights assertsd in connection with any item mentionedTn this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement cf such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee end must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ol this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. i 1. he fo re - al \ at th at at \ 2. n y '\ S t jf g Ia .'i,j | b 1 S 1'! t; .t;- 266 DUP050297449  can be andards : prepa- Designation: D 2201 - 65 (Reapproved 1S7)e1 Standard Test Method for Preparation of Hot-Dipped Nonpassivated Galvanized Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products1 This standard is issued 'under the fixed designation D 2201; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearoflast revision. A number in parenthesesindicates the year oflast reapproval. A superscript epsilon, (c) indicates an editorial change since the last revision or reapproval. ei N01' --Footnote i- and Note 4 were corrected editorially in October. 1987. 1. Scope 1.1 This test method describes the preparation of a type of hot-dipped, nonpassivated, galvanized steel panel to be used for testing paint, varnish, lacquer, conversion coatings, and related products. 1.2 This standard may involve hazardous materials, oper ations, and equipment This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: A 525 Specification for General Requirements for Steel Sheet, Zinc-Coated (Galvanized) by the Hot-Dip Process2 D2092 Practice for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Painting3 2.2 U.S. Federal Test Specifications: 0-T-634a Type II Trichloroethylene4 O-P-191 a Perchloroethylene4 3. Test Panels 3.1 The test panels shall be prepared from galvanized sheet that has not been subject to any kind of treatment for the purpose of passivating (Note 1) and shall be completely free from any visible signs of storage stain or white rust. The gage shall be No. 20 (0.0396 in.) (1 mm) unless otherwise agreed upon between the manufacturer and the purchaser, but in no case lighter than No. 24 gage (0.0276 in.) (0.7 mm). The galvanizing shall be of the 1.25-oz class conforming to Specification A 525, known as "commercial (full spangle)." N23' 1--This test panel is designed for referee testing and is not typical of galvanized material normally stocked in commercial ware ' This test method is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.27 on Accelerated Testing. Current edition approved Aug. 31, 1965. Originally published as D 2201 - 63 T. Last previous edition D 2201 - 65 (1981 )CI 1 Annual Book ofASTM Standards, Vol 01.06. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Available from Standardization Documents Order Desk, Bldg. 4 Section-D, 700 Robbins Ave., Philadelphia, PA 19111-5094. houses. Specified panels may be obtained from standard panel suppliers. 3:2 The zinc coating shall have been applied by a contin uous galvanizing method, using an aluminum-bearing zinc. Galvanized steel is customarily shipped from the mills unoiled; however, galvanized steel that has been oiled with a nonreactive rust preventative oil shall be acceptable under this specification. 3.3 After cutting, the panels shall be cleaned in organic solvents or vapor degreased and wrapped in clean paper having a neutraFpH and sealed in vappiproof bags or envelopes. The use of alkali cleaners shall not be permitted. The panel size shall be not less than 23A by 5% in. (70 by 150 min) and all comers and edges shall.be smooth and uniformly rounded. 4. Solvents and Reagents 4.1 Solvent Mixture--Prepare a solvent mixture con sisting of either equal volumes of Varnish Makers' and Painters' (VM&P) naphtha and xylene or of 3 volumes of VM&P naphtha and 1 volume of ethylene glycol monoethyl ether (2-ethoxyethanol). 4.2 Stabilized Trichloroethylene or Perchloroethylene. N45' 2--Perchloroethylene and trichloroethylene shall conform to and be maintained in accordance with the Federal Specification for Trichloroethylene (0-T-634a Type II) or Perchloroethylene (0-P-191a). 5. Procedure A--Galvanized Steel Test Panels Without Chemical Treatment 5.1 Wipe the corrosion-free panels vigorously on both sides with a cloth wet with the solvent to remove the gross film of oil. Clean the panels by either solvent spray or vapor degreasing, as described in 4.2 and 4.3. 5.2 Solvent Spray Cleaning--Spray the solvent mixture (3.1) downward at an acute angle to the panel surface using a spray gun operated with the fluid tip wide open and the atomizing tip almost completely closed. Preferred practice is to support the panels on a rack at an angle of approximately 25 from the vertical and to hold the spray gun so that the jet is directed vetically downward. The bottoms of the panels should rest upon projections, such as nails, which permit the solvent to drain from the bottom edge. Direct the solvent over the surface of the panel in an oscillating rinsing manner, moving the spray progressively from the top to the bottom of the panel until all soluble and loosely adhering soil has been washed off. The minimum treatment shall consist of five JL-. 267 DUP050297450 D 2201 washings, three on the side to be tested, and two on the reverse aide. Alternate the washings, starting and ending with the side to be tested. Allow the panels to dry at room temperature until all solvent has evaporated (approximately 15 min). Then rub the panels briskly with a clean, lint-free cloth to remove any adhering dirt or smut. Place the panels in an oven and uniformly heat at 350F (177C) for 10 min. After heating, remove the panels from the oven, allow them to cool to room temperature, and coat them immediately with the paint system (Note 3). Do not touch the panels with the fingers during the entire process of preparation. N67' 3--Unpainted panels that have been stored for long periods may cause fine blisters to form on paint, usually at the zinc spangle boundaries, and baking the panel as described eliminates this blistering. 5.3 Vapor Degreasing--Suspend the panels in a vapor phase-type degreaser containing stabilized trichloroethylene or percMoroethylene and allow them to remain above the boiling solvent until they attain the temperature of the vapor, at which time condensation on the panels no longer occurs. Allow the panels to cool to room temperature and rub briskly with a clean, lint-free cloth. Place the panels in an oven and uniformly heat at 350F (177C) for 10 min. After heating, remove the panels from the oven, and allow them to cool to room temperature and coat them immediately with the paint system (Note 3), Do not touch the panels with the fingers during the entire process of preparation. I 6. Procedure B--Galvanized Steel Test Panels with Chem ical Treatment 6.1 Clean standard, corrosion-free panels, without sanding or abrasion, in accordance with Procedure A. Coat : the panels with b phosphate coating or other conversion coating representative of production performance (Note 4), The conditions of treatment shall be agreed upon between the manufacturer and the purchaser. Paint the treated panels immediately or store in a vacuum desiccator until needed. If panels are stored in a vacuum desiccator, upon removal from the desiccator, place the panels in an oven and uniformly 1 heat at 350F (177C) for 10 min. After heating, remove the panels from the oven, allow them to cool to room tempera ture, and coatthem immediately with the paint system (Note 3). Do not touch the panels with the fingers during the entire : process of preparation. I N89' 4--In the selection of these types, refer to Practices D 2092. I The American Society tor Testing amt Msterlala takes no poaMon respecting the validity of any patent rights assorted In connection with any Item mentioned In thl8 standard. Users ot this standard an expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. 1. Sc 1.1 for te 1.2 prodi as a r 1.3 probl user heali limiti 2. R* This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every rive years and H not revised, eitherreepproved or withdrawn. Your comments an Invited either lor revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Pace St., Philadelphia, PA 19103. 2.1 c: Df 1 D D D ": D D D D ,j D ' | D I D < 1T Relate D0I.4 Cur publis *A *A ' i i 6A 268 mi DUP0502 97451 mn. After w them to ately with !s with the ith Cheat. without e A. Coat onversiou (Note 4). < between ted panels needed. If oval from uniformly :move the temperatem (Note the entire s D 2092. Designation: D 2205 - 85 (Reapproved 1990)e1 Standard Guide for Selection of Tests for Traffic Paints1 This standard is issued under the fixed designation D 2205; the number immediately Mowing the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. el N:;' --Sections 12 and 13 were editorially changed in March 1990. Scope 1.1 This guide covers the selection and use of procedures for testing traffic paints in the laboratory and in the field. 1.2 This guide covers the testing of a ready-mixed paint product of sprayable consistency that shall be suitable for use as a reflecting traffic guide on paved roadways. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: C 219 Terminology Relating to Hydraulic Cement2 D8 Terminology Relating to Materials for Roads and Pavements3 D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products4 D154 Guide for Testing Varnishes3 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints6 D215 Methods of Chemical Analysis of White Linseed Oil Paints5 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer5 D 711 Test Method for No-Pick-Up Time of Traffic Paint5 D713 Practice for Conducting Road Service Tests on Fluid Traffic Marking Materials5 D 868 Test Method for Evaluating Degree of Bleeding of Traffic Paint5 D 869 Test Method for Evaluating Degree of Settling of. Paint5 D 870 Practice for Testing Water Resistance of Coatings Using Water Immersion5 D913 Test Methods for Evaluating Degree of Resistance to Wear of Traffic Paint5 1 This guide is under the jurisdiction of ASTM Committee EM on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.44 on Traffic Coatings. Current edition approved Dec. 13, 1985. Published March 1986. rOiiginally published as D 2205 - 63 T. Last previous edition D 2205 - 75. 2 Annual Book ofASTM Standards, Vol 04.01. 3 Annual Book ofASTM Standards, Vols 04.02 and 04.03. 4 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06,03. 3 Annual Book ofASTM Standardsr Vol 06.01. 6 Annual Book ofASTM Standards, Vols 06.01 and 06.02. D968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive5 D969 Test Method for Laboratory Determination of Degree of Bleeding of Traffic Paint5 D 1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems5 D1309 Test Method for Settling Properties of Traffic Paints During Storage5 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products5 D1644 Test Methods for Nonvolatile Content of Varnishes5 D1647 Test Methods for Resistance of Dried Films of Varnishes to Water and Alkali5 D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials7 D 1737 Test Method for Elongation of Attached Organic Coatings with Cylindrical Mandrel Apparatus8 D 2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates5 D2371 Test Method for Pigment Content of SolventReducible Paints5 D2372 Method of Separation of Vehicle from SolventReducible Paints3 D4061 Test Method for Retroreflectance of Horizontal Coatings7 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry8 E 308 Method for Computing the Colors of Objects by Using the CIE System8 2.2. U.S. Federal Test Methods Standard 141B:9 4121 Dry Opacity 3. Terminology 3.1 Definitions--For definitions used in this guide, refer to Terminology C 219 and Definitions D 8 and D 16. 4. Summary of Guide 4.1 This guide consists ofthe following tests that, although not exhaustive, cover the areas normally of concern in traffic paint testing: ''Annual Book ofASTM Standards, Vol 14.02. 8 Discontinued; see 19S3 Annual Book ofASTM Standards, Vol 06.01. 9 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 269 __ DU PO 502 97452 Liquid Paint Properties Application and Appearance Properties Properties of the Dried Film Analysis of Paint Field Evaluations Sections 6 through 1L 12 through 17 IS through 20 21 through 24 25 through 29 5. Conditions Affecting Traffic Paint 5.1 Practical requirements for traffic paint may vary with: 5.1.1 Substrate type, such as Portland cement and as phaltic concretes, and the various coarse aggregates used therein. 5.1.2 Climatic conditions, both generally and specifically, at the time of paint application. 5.1.3 Service density, such as heavy traffic areas in cities versus lightly traveled rural highways and parking lots. 5.1.4 Traffic type, whether light passenger cars or heavy trucks and airplanes. 5.1.5 Presence of foreign matter on the road surface, such as oil, old paint, skid marks, sand, salt, concrete curing compound, etc. 5.2 New Portland cement concrete surfaces have a greater degree of moisture and alkalinity than older surfaces and thereby adversely affect paint adhesion. Paint adhesion is also affected by the ratio of cement to fine aggregate, coarse aggregate, and mixing water, as well as by the surface character of the aggregate that can range from impervious smooth quartz to irregular, porous slag. LIQUID PAINT PROPERTIES 6. Skinning 6.1 Paints containing a binder that dries by oxidation are subject to skin formation in a partially filled can or by diffusion of air into a filled can. Since skins are insoluble in the paint they must be removed before use. The referenced test employs a partially filled container to indicate the tendency of a paint to skin. A typical minimum time for skinning is 18 to 24 h. 6.2 Examine the original sample for skins both on the surface and in the mass. Using a well-mixed, skin-free portion of the sample, perform a skinning test in accordance with Guide D 154, except use a 1-pt (0.5-L) friction-top can instead of an- 8-oz (0.25-L) jar. 7. Coarse Particles 7.1 Paints must be free of oversize particles and foreign matter to avoid dogging application equipment, a typical maximum being i % by weight of total paint. The referenced test with a 325-mesh (45-p.m) screen gives the percent of this material in the paint. 7.2 Determine coarse particles in accordance with Test Methods D 185. N<=' 1--This test is not used for traffic paint containing pre-mixed glass beads. 8. Fineness of Dispersion 8.1 The more finely a pigment is dispersed, the more efficiently it is being used. One method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the material down a calibrated, tapered groove in a hardened steel block with the groove varying in depth from 4 to 0 mils (100 to 0 pm). The point at which continuous groupings of particles or agglomerates, or both protrude through the surface of the liquid is taken as the fineness reading. Lower readings in mils or micrometres or | higher reading in Hegman units indicate better fineness of ' dispersion. 8.2 Fineness of grind is not generally specified for traffic paint but some application equipment may require a limit of 1 to 2 Hegman units (3 to 3.5 mils, 75 to 90 pm), if additional assurance is needed that the paint will not clog application equipment, determine the fineness in accordance with Test Method D 1210 after reducing the traffic paint with mineral spirits, or compatible aromatic solvent with a similar evaporation rate, to keep the film wet long enough to determine the end point more easily. When a premix traffic paint is being tested, conduct the test on the paint before addition of the beads. 9. Density or Weight per Gallon _ 9.1 Density as measured by weight per unit volume is not a performance characteristic but is used to check product uniformity from batch to batch. A calibrated weight per gallon cup is used. 9.2 For an unbeaded paint, determine the density in accordance with Test Method D 1475. 9.3 For beaded paints, use a special weight-per-gallon cup7108having a modified cap so that the beads do not interfere with a snug fit of the cap to the cup. Proceed in accordance with Test Method D 1475. 10. Consistency 10.1 Paints of a given type should fall within a stated consistency range as agreed upon between the purchaser and the seller. Consistency is used mainly to ensure product uniformity. Improper consistency, however, can adversely affect application properties, and in turn, paint performance. 10.2 Determine consistency using the Stormer viscometer in accordance with Test Method D 562. If the requirement is in Krebs units, Table 1 of Test Method D 562 permits changing seconds to KU. 11. Package Stability 11.1 Since paints are not normally used immediately after manufacture, they must remain stabje in the can for some time, which for traffic paints does not generally exceed 6 months. Although package stability can usually he deter mined by alternatively heating and cooling a specimen, occasionally the results do not coincide with storage at normal temperature. The referenced methods determine the degree of pigment settling after 2 weeks cycling or after 6 months storage at room temperature. These are usually sufficient as it is difficult to rate numerically the ease of redispersing an aged traffic paint. 11.2 Determine the degree of pigment settling in the accelerated test in accordance with Test Method D 1309. Determine the degree of pigment settling and ease of 10 A satisfactory modified cup is available from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. j-grnixi fvfetho 12. Dr 12.1 import opened transfe: 12.2 Methai tion, it 13. Bli 13.1 as bitu paint f compat paint, arbitrar bleedin. in acco. 14. Hit 14.1 a paint thickne: flow am 14.2 accorda Test Me in ASTf 15. Col. 15.1 means c not usu: standan can be c than for fast and obtainec sensitive subseqm 15.2 I tristimul with Me 15.3 .1 against s D 1729. 270 DUP050297453 D 2205 h ^mixing a shelf-aged specimen in accordance with Test instrumental measurement of small color differences observ Method D 869. ie >r APPLICATION AND APPEARANCE PROPERTIES able in daylight illumination between nonfluorescent, nonmetameric, opaque surfaces. 16. Reflectance j2. Drying Time 16.1 Reflectance is a measure of the light reflected from ic 12.1 The drying time of a traffic paint is particularly the surface of a paint. It determines which of two specimens )f important because it determines how quickly a lane can be appears lighter when viewed in average daylight at an angle If opened to free flow of traffic without the paint being that eliminates gloss effects. >g tjansferred to adjacent pavement. 16.2 Determine the green filter reflectance in accordance 12.2 Though no-pick-up time as determined by Test with Test Method E 97. n Method D 711 has no direct correlation with field applica- a jion, it is employed as a quality control test. 17. Night Visibility or Retroreflectance of Beaded Paints at o Low Angles ic e 13. Bleeding 13.1 Bleeding refers to the passage of colored matter such 17.1 This property is important to traffic paint but visibility at night is not related to daylight reflectance. The as bitumen from an asphalt pavement through the traffic retroreflectance evaluation of test panels coated with traffic paint film. It is a function of the age of the asphalt, its paint should be in accordance with Test Method D4061. compatability with the paint, and the speed of drying of the Such panels can serve as controls in monitoring the applica n :t :r paint. Typical traffic paints give results of 6 to 10 on an arbitrary scale of photographic standards where 10 is no bleeding and 2 is considerable bleeding. Determine bleeding io accordance with Test Methods D 868 and D 969. tion of traffic paint and can be helpful in correlating visual ratings with absolute values. PROPERTIES OF THE DRIED FILM n 14. Hiding Power 18. Resistance to Wear n 14.1 Hiding power or opacity is a measure of the ability of 18.1 Resistance to wear is a measure of the ability of the >t a paint to hide the substrate. It varies, naturally, with the dried film to withstand wear from traffic and from objects n thickness of the applied film that may be influenced by the rolled or pulled across the surface. In the referenced method flow and application properties of the paint. abrasive is poured onto a dry film on a glass panel until the 14.2 Determine the dry hiding power of traffic paints in paint is removed. A typical value for traffic paint is 65 L of accordance with Procedure A, Method 4121 of U.S. Federal sand for removal of a 3-mil (75-pm) dry film. Determine Test Method Standard 141B. (This method is being rewritten resistance to wear in accordance with Test Method D 913. d in ASTM form.) 18.2 Using unbeaded traffic paint, determine the abrasion d resistance to falling sand or silicon carbide in accordance n 15. Color and Color Difference with Test Methods D 968. y 15.1 The color of a paint may be determined precisely by means of a spectrophotometer. However, the exact color is 19. Elongation :r is 'S not usually as important as how closely a paint matches a standard. Color difference between a product and a standard can be determined visually or with less elaborate instruments 19.1 Elongation is a measure of the flexibility of a paint film. Traffic paints may have difficulty in meeting the referenced test if they are over-pigmented to obtain high than for color measurement. Visual comparison of color is reflectance. fast and often acceptable although numerical values are not 19.2 Using unbeaded traffic paint, determine the flexi obtained. Color difference instruments, while not more bility in accordance with Test Method D 1737 but using sensitive than the eye, provide numerical values that can be 30-gage (0.32-mm) tin plate in place of the specified steel subsequently compared to later measurements. panel. 15.2 If required, determine the color in terms of 19.2.1 As the thickness and curing conditions are not tristimulus values or chromaticity coordinates in accordance specified in Test Method D 1737, one of the following h it with Method E 308. alternatives should be used for testing traffic paint: 15.3 Determine color difference by visual comparison 19.2.1.1 Apply a 15-mil (380-p.m) wet film, allow to air ie against standard color chips" in accordance with Practice dry 18 h, bake 2 h at 50"C, and let cool before conducting the 6 D 1729. This practice covers the spectral photometric, and test with a Vi-in. (12;7-mm) mandrel. iy )f Seometric characteristics of light source, illuminating and viewing conditions, size of specimens, and general proce 19.2.1.2 Apply a 10-mil (250-pm) wet film, allow to air dry 24 h, bake 1 h at 65C, cool, and use a `A-in. (6.4-mm) dures to be used in the visual evaluation of color differences mandrel. ie of opaque materials. 19.2.1.3 Apply a 6-mil (150-pm) wet film, bake 6 h at 9. 15.4 Determine color difference instrumentally in accord 100C, cool, and use a 'A-in. (6.4-mm) mandrel. >f ance with Test Method D2244. The method covers the 20. Water Resistance Standard yellow color chips may be obtained from the Traffic Control Osteins Div., HTO-20, Office of Traffic Operations, Federal Highway Adminis- astion, Washington, DC 20590. 20.1 This property is important to traffic paints because they are frequently exposed to rain or condensation on bridges. The immersion test time is quite short in relation to 271 DUPO 502 97454 # D 2205 actual exposure so that the test detects only paints with poor water resistance. 20.2 Using unbeaded paint, determine water resistance in accordance with either Practice D870 or Test Methods D 1647. 20.3 As Practice D 870 specifies steel panels but not the immersion time, while Test Methods D 1647 requires tin plate and an immersion of 18 h, the following should be used fortesting traffic paint: apply a 5-mil (130-pm) wet film to a clean glass panel, allow to air dry for 72 h, immerse in reagent water for 24 h, and allow a recovery period of 2 h before examining. ANALYSIS OF PAINT 21. Chemical Analysis 21.1 If a specification requires certain raw materials or certain components in a given amount, then chemical analysis is necessary to determine whether the specified materials are present in the required amounts. Analysis does not necessarily establish paint quality that can also be greatly affected by manufacturing techniques. Select test procedures from Methods D2I5 and other ASTM methods that are pertinent to the components of traffic paints. N>?' 2--No single schematic analysis is comprehensive enough to cover the wide variety of traffic paint compositions. 22. Nonvolatile Content (Paint) 22.1 The percent nonvolatile matter indicates the amount of material remaining after the solvent evaporates and is a measure of the film solids. Determine the nonvolatile content in accordance with Test Methods D 1644 using a larger specimen size in the case of beaded paint. It is suggested that the methods be selected as follows: 22.1.1 Test Method A--3 h at 105C for paints where the nonsolvent components decompose at 149C, and 22.1.2 Test Method B--10 min at 149C for most paints where the nonsolvent components are reasonably stable at 149C. 23. Pigment Content 23.1 Pigment gives paint its hiding and color and influ ences many other properties. Determine the percent pigment in accordance with Test Method D 2371. 24. Binder Content 24.1 The nonvolatile vehicle is that portion of the filmforming solids in a paint other, than the pigment. It is not to be confused with the nonvolatile portion of the vehicle. Subtract the pigment content from the nonvolatile content to obtain the nonvolatile vehicle content. Ifdesired, separate the vehicle for further analysis in accordance with Method D2372. FIELD EVALUATIONS 25. Road Service Test 25.1 Whereas numerous laboratory tests in the previous sections indicate general suitability of traffic paint, and also batch-to-batch uniformity, these tests cannot predict per. formance under all possible end uses. Accordingly, the test paint should be applied in a repeatable manner under carefully stated conditions of end use and then tested observed, and evaluated at stated times throughout the usefoj life of the paint 25.2 Proceed in accordance with Practice D713, being careful to record the value of each variable stated. 26. Retroreflectance 26.1 Since there is no acceptable instrumental method of evaluating the retroreflectance in the field of the glass spheres on (in) the traffic paint stripe (Note 4), the following two visual methods are extensively used: (/) rating longitudinal stripes from a car traveling at approximately 20 to 35 mph and requiring a test line 50 ft (15 m) long, and (2) rating transverse test stripes in the wheel tracks with tungsten illumination from' the side of the road with eye and light source (held chest high) and separated by a distance that corresponds to the observation angle of a driver viewing the stripes on a highway. 26.1.1 These ratings are based on a scale of 10 (complete (100 %) retroreflectance) to 0 (no retroreflectance). N@A' 3--The wheel track is the area extending 9 in. (230 mm) to each side of the point of greatest wear. N@A' 4--An instrumental method with much greater precision & being developed. 27. Durability 27.1 The test line rating is based on the paint film remaining at the time of inspection when estimated by dose observation with the unaided eye. The rating is on the scale from 0 to 10, the latter representing 100 % remaining, a rating of 9 representing 90 % remaining, etc. 28. Appearance 28.1 This is the complete impression conveyed when the test stripe is viewed at a distance of at least 10 ft (3 m). Any discoloration of the surface due to bleeding, dirt collection, darkening, fading, mold growth, etc. will affect the rating that is also on the scale from 10 to 0. ; 29. Length of Useful Life 29.1 The length of useful life is the length oftime (in days) between application of the test fines and when the weighted rating first reaches a value of 4, or when any specific quality (appearance, durability, or night visibility) first reaches the numerical rating of 3, whichever is the lesser number of days. 29.2 When it is necessary to calculate the "length ofuseftil life," calculate as follows (Practice D 713): L = D x (10 -- 4)/(10 - R) = 6D/(10 - R) ) where: L = length of useful life, D -- number of days the test stripe has been on the road, and R = weighted rating at time of calculation. j i j j i 272 DUP050297455 and also Jict per. the test r under \ tested, he useful 3, being method of s spheres ving two gitudinai 35 mph 2) rating tungsten md light nee that wing the complete 10 mm) to recision is lint film by close the scale aining, a when the m). Any Election, e rating 'in days) weighted ic quality iches the r of days, of useful the road, # D2205 The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users at this standard are expressly advised that determination ot the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every fire years and if not revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standerdor tor additional standards and should be addressed to ASTM Headquarters. Your comments win receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103, 273 DUP050297456 <1 Designation: D 2243 - 90 Standard Test Method for Freeze-Thaw Resistance of Water-Borne Coatings1 This standard is issued under the fixed designation D 2243; the number immediately following the-'designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 3012 ofFederal Test Method Standard No. 141 andfor listing in the DoD Index ofSpecifications and Standards. : 7. Repoi 7.1 R( accordan 7.2 Rt mens, ar with 6.2. 7.3 Rt teristics c : 6.3. 1. Scope are applied promptly to the cans to prevent evaporation 1.1 This test method covers the determination of the losses. Two such specimens are required for each test extent to which water-borne coating retain their original properties free of detrimental changes. 1.2 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility ofthe user ofthis standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 5. Exposure to Test Conditions 5.1 Store one can at room temperature and identify this as the control specimen. 5.2 Place the second can, the paint under test, identified as the "test specimen", in the chamber maintained at 0"F (-18C) in such a manner that it does not touch the walls or 2. Referenced Documents 2.1 ASTM Standards: D 562 Test Method for Consistency of Paints Using the Stormer Viscometer2 D2196 Test methods for Rheological Properties of Non- Newtonian Materials By Rotational (Brookfield) Viscometer2 bottom of the chamber and so that free circulation of air around it is permitted. The placing of cans on racks that raise them off the bottom of die chamber or upon pieces of insulating board resting on the bottom is suggested. In the case of several test specimens, maintain a minimum of 1 in, (25 mm) of air space between adjacent cans and between cans and the chamber walls. Keep the test specimen in the chamber for 17 h and then remove and allow to stand for 7 h I \ ' I \. 3. Apparatus 3.1 Test Chamber--A suitable cabinet, room, or enclo sure space large enough to contain the specimens to be tested permitting at least 1 in. (25 mm) of air space between the sides of adjacent cans and capable of being maintained undisturbed at room temperature, adjacent to the control specimen, for a complete freeze-thaw cycle of 24 h. 5.3 Repeat 5.2 for additional freeze-thaw cycles, as many as agreed on between cooperating laboratories or buyer and seller (One to five cycles are usual.). ; S 1 \ continuously at a temperature of 0F (--18C). NBC' I--Although a variation of the test chamber temperature of 3.5F (2C) is allowed, the test chamber temperature should be maintained as near 0F (--18C) as practicable and the amount of variation should be recorded and reported! 6. Examination 6.1 After completion of the agreed or specified number of cycles, before stirring, examine both specimens for condition in the can, observing and rating any evidence of settling, 3.2 Viscometer--A Stormer viscometer with paddle type rotor as described in Test Method D 562 or a Brookfield viscometer as described in Test Methods D 2196. 3.3 Test Charts--Smooth surface paper charts having adjacent black and white areas, and coated with a suitable gelation, coagulation, lumpiness, etc. as slight, moderate or pronounced. 6.2 Then stir the specimens and determine their viscosi ties in accordance with Test Method D 562 or Test Methods D 2196, and record the temperature of measurement. varnish or lacquer to render the surface impermeable to paint liquids. 3.4 Paint Brush, 1 in. (25 mm). 4. Preparation of Sample and Specimens NDE' 2--Stir specimens by hand in their can using a stainless sted paint spatuia with a blade measuring approximately 5 by % in. (125 bj 20 mm). Stir carefttlly so as to avoid air entrainment and Foam. NDE' 3--In carrying out consistency determinations using Tei Method D 562, specimens should be maintained in 77F (25"C) uad f | 4.1 Prepare specimens for testing by filling 1-pt (500 mL) resin-lined, friction-top cans two thirds full. Ensure that the two successive readings agree within 5 g. As is the case with ii non-Newtonian fluids, viscosity variation is dependent to a degree upct intensity and duration of agitation. Utmost care should be taken that bulk sample from which the cans are filled is well stirred and control and test specimens receive identical treatment dining all strains uniform, that the containers used are clean, and that the lids operations. | 6.3 Immediately following the viscosity determinations I 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint apply both specimens of paint to a test panel (3.3) by mean* and Related Coatings and Materials and is the direct responsibility of Subcom of a clean 1-in. (25-mm) brush. Allow to dry at least 24 fc a mittee EX) 1.42 on Architectural Finishes. Current edition approved Oct. 26. 1990. Published December 1990. Originally published as D 2243 - 64 T. Last previous edition D 2243 - 82 (1987}ei. then compare the test specimen with the control. Note afll changes in hiding power, gloss, speckiness, agglomeration 2 Annual Book ofASTM Standards, Vol 06.01. l coagulation, or color as slight, moderate or pronounced. 274 DU PO50297457 /aporation test. itifythisas identified red at 0F he walls or tion of air s that raise pieces of ted. In the tm of 1 in. d between nen in the and for 7 h he control h. s, as many buyer and D 2243 7. Report 7.1 Report on the condition of the paint in tbe can, in accordance with 6.1. 7.2 Report the viscosities of the test and control speci mens, and the temperature of measurement, in accordance with 6.2. 7.3 Report comparatively on the visible dry film charac teristics ofthe test and control specimens, in accordance with 6.3. 8. Precision 8.1 The precision of this test method in regard to viscosi ties is as specified in Test Methods D562 or D2196, whichever is employed. 8.2 No precision statement is made in regard to the other properties, because of the subjective nature of the observa tions. 9. Keywords 9.1 freeze-thaw resistance; package stability The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. a ag, e or viscosiMethods ;nt. rainless steel '4 in. (125 by foam. ; using Test (25"Q until rase with all . degree upon je taken that ng all stirring rminatiotis, ) by means least 24 h, 1. Note any iomeration, aunced. 275 DUP050297458 4 Designation: D 2244 - 89e1 Standard Test Method for Calculation of Color Differences From Instrumentaily Measured Color Coordinates1 This standard is issued under the fixed designation D 2244; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. l NFG' --Superscript for if in 6.4 was editorially corrected in December 1990. INTRODUCTION 3.2.1 directic stimuli coordir a sped! 4. SH< I 4.1 ' spedm of a sp ings fix to colo directly compu from d the per test sp< This test method originally resulted from the consolidation ofa number of separately published methods for the instrumental evaluation of color differences. As revised in 1979, it included four color spaces in which color-scale values could be measured by instruments, many of which were obsolete, and the color differences calculated by ten equations for different color scales. The sections on apparatus, calibration standards and methods, and measurement procedures served little purpose in the light of modem color-measurement technology. The present revision omits these sections, and limits the color spaces and color-difference equations considered, to the three most widely used in the paint and related coatings industry. 1 ; ; 1. Scope 1.1 This test method covers the calculation, from instru mentaily measured color coordinates based on daylight illumination, of small color differences between nonfluorescent, nonmetameric, opaque specimens such as painted panels. (Where it is suspected that the specimens may be metameric, that is, possess different spectral curves though visually alike in color, Practices D 1729 and D 4086 should be used to verify instrumental results.) The color differences determined by these procedures are expressed in terms of approximately uniform visual color perception in CIE 1976 CIELAB opponent-color space (l),2 Hunter LH, a^, bH opponent-color space (2), and the Friele-MacAdam-Chickering (FMC-2) color space (3). 1.2 For product specification, the permissible color differ ence between test specimen and reference and the procedure for calculating the color difference shall be agreed upon by the purchaser and the seller. Specific color tolerances may be required for each material and condition of use since other appearance factors (for example, proximity, gloss, and tex ture) may affect the correlation between the magnitude of a measured color difference and its commercial acceptability. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.26 on Optical Properties. Current edition approved Oct. 27, 1989. Published December 1989. Originally published as D 2244 - 64 T. Last previous edition D 2244 - 85. 2 The boldface numbers in parentheses refer to the list of references at the end of this method. appropriate safety and health practices and determine the ' applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1729 Practice for Visual Evaluation of Color Differences of Opaque Materials3 D3964 Practice for Selection of Coating Specimens for Appearance Measurements4 D 4086 Practice for Visual Evaluation of Metamerism3 E 179 Guide for Selection of Geometric Conditions for Measurement of Reflection and Transmission Proper ties of Materials3 E 284 Definitions of Terms Relating to Appearance of Materials3 E 308 Method for Computing the Colors of Objects by Using the CIE System3 [ j [ j j 3. Terminology \ j 3.1 Definitions--For the following definitions as well as ! for other definitions of terms used in this test method, see [ Definitions E 284: tristimulus values, chromaticitycoordi* | nates, and opponent-color scales. S 3.2 Description of Term Specific to This Standard: \ 3.2.1 color difference: \ 3.2.1.1 color difference (perceived)--the magnitude and character of the difference between two colors described by i such terms as redder, bluer, lighter, darker, grayer, or j cleaner. f 3 Annua/ Book ofASTM Standards, Vol 14.02. 4 Annual Book ofASTM Standards> Vol 06.01. j 5. Sigi 5.1 values nonun values degree region: the ot specim likely > among obtain factor in one of spet 5.2 1976 t CIEL/ has fc indust of the still u becau` pretin. methc 5.3 systeir nents whetha stan< necess from Inforn includ comp; 5.4 values of the satura 6. De 6.1 276 DU P050297459 JufSitt I D 2244 mine the ifferences mens for terism3 itions for Properranee of ejects by as well as ethod, see ty coordiird: itude and scribed by grayer, or 3.2.1.2 color difference (computed)--the magnitude and ijfection of the difference between two psychophysical color jjnuli defined by tristimulus values, or by chromaticity c0ordinates and luminance factor, as computed by means of specified set of color-difference equations. Summary of Test Method 4, l The differences in color between a reference and a test specimen are determined from measurements made by use 0f a spectrophotometer or a colorimeter. Reflectance read- from such instruments are converted by computations color-scale values, or these color-scale values may be read directly from instruments that automatically make the imputations. Color-difference magnitudes are computed, j.0m differences in these color-scale values, that represent jpc perceived color differences between the reference and the test specimen. 3, Significance and Use 5.1 The original CIE color scales based on tristimulus values X, Y, Z and chromaticity coordinates x, y are visually nonuniform. Each subsequent color scale based on CIE values has had weighting factors applied to provide some degree of uniformity so that color differences in various regions of color space will be more nearly comparable. On the other hand, color differences obtained for the same specimens evaluated in different color-scale systems are not likely to be identical. To avoid confusion, color differences among specimens should be compared only when they are obtained for the same color-scale system. There is no simple factor that can be used to convert accurately color differences in one system to differences in another system for all colors of specimens. 5.2 For uniformity of practice, the CIE recommended in 1976 the use of two new improved color scales, of which the CIELAB scale, with its associated color-difference equation, has found wide acceptance in the coatings and related industries. However, it has not completely displaced the use of the Hunter LH, aH, bH and the FMC-2 scales, which are still utilized to allow comparison with earlier results and because of their familiarity to those responsible for inter preting them. Therefore, all three scales are included in this method as the most widely used in industrial laboratories.. 5.3 Users of color differences have found that, in each system, summation of three vector color-difference compo nents into a single scalar value is useful for determining whether a specimen color is within a specified tolerance from t standard. However, for control of color in production, it is tecessary to know not only the magnitude of the departure a standard but also the direction of this departure. Information on the direction of a color difference is easily included by giving the three instrumentally determined w>mponents of the color difference. 5.4 Selection of color tolerances based on instrumental 'dues should be carefully correlated with a visual appraisal the acceptability of differences in hue, lightness, and saturation obtained by using Practice D 1729. Description of Color-Difference Equations 6.1 CIE 1931 and 1964 Color Spaces--The daylight colors of opaque specimens are represented by points in a space formed by three rectangular coordinates representing the lightness scale Y and chromaticity scales x and y, where: X x~X+V+Z Y ymX+T+Z Y= Y where X, Y, and Z are tristimulus values for either the 1931 CIE standard observer (2observer) or the 1964 CIE supple mentary standard observer (10 observer) and standard illuminant C, D6S, or another of daylight quality. These scales do not provide a perceptually uniform color space! Consequently, color differences are seldom if ever computed directly from differences in x, y, and Y. 6.2 CIE 1976 L* a* b* Uniform Color Space and ColorDifference Equation (1, 4>--This approximately uniform color space' is a simplified version of the Adams-Nicker$oii color-scale system (5-7), It is produced by plotting in rectangular coordinates the quantities L*, a*, b*, calculated as follows: 1* = ii6(y/y,,)`A- 16 a* = SQ0[{XjX,,)'h - (Y[Y,,n b* = 200107 - {ziznr\ X/Xn; Y/Y,,; ZjZn > 0.01 The tristimulus values X,,, Y,,, Zn define the color of the normally white object-color stimulus. Usually, the white object-color stimulus is given by the spectral radiant power of one of the CIE standard illuminants, for example, C, D6S or another of daylight quality, reflected into the observers eye by the perfect reflecting diffuser. Under these conditions, X,,, Y,,, Z,, are the tristimulus values of the standard illuminant with Y,, equal to 100. 6.2.1 The total difference AE%, between two colors each given in terms of L*, a*, b* is calculated as follows: AE% =[(AI*)2 + (Aa*)2 + (Ab*?f> NJK' 1--The color space defined above is called the CIE 1976 L* a* b* space and the color-difference equation the CIE 1976 L* a* b* color-difference formula. The abbreviation CIELAB is recommended. 6.2.2 The CIE 1976 (L* a* b*) space fails to approximate uniform color spacing when one or more of the ratios xjxm Y/Y,,, and Z/Z,, is less than 0.01. In calculating L*, values of Y/Y,, less than 0.01 may be included if the normal formula is used for values of Y/Y,, greater than 0.008856, and the following modified formula is used for values of Y/Y,, equal to or less than 0.008856. l * = 903.3( y/ y,,) y/ y,, < 0.008856 6.2.3 In calculating a* and b*, values of XjX,, Y/Y,,, ZfZ,, less than 0.01, may be included if the normal equations are replaced by the following modified equations for ail calculations of a* and b*: a* = 500[/OTO -f(Y/Yn)] b* = 200[/(y/y,,)-KZjZfo where: f{X/X,,) = {XjX^ ' f{X/X,,) = 7.7i7(X/X,,) + 16/116 f(Y/Yn) = (y/y,,r X/X,, > 0.008856 X/X,, < 0.008856 y/y,, > o.oossse ji DU PO 502 97460 0 2244 /(7/7,,) = 7.787(7/7,,)+ 16/116 /(Z/ZJ = (Z/Z,,)'/! /(Z/Z,,) = 7.787(Z/Z,,) + 16/116 '7/7,, <0.008856 Z/Z,, > 0.008856 Z/Z,, 0.008856 NLM' 2--To compare values of A.E(.4/V40) calculated by means of the Adams-Nickerson (+A'40) equation with AE*^, multiply AE(AN40) values by the factor 1.1 to facilitate the comparison. 6.2.4 The magnitude, AE*ab, gives no indication of the character of the difference since it does not indicate the relative quantity and direction of hue, saturation, and lightness differences. 6.2.5 The direction of the color difference is described by the magnitude and algebraic signs of the components AL*, Aa*, and A b*: AL* = Lf - IS Aa* = at - a* Ab* = b* -- b% where L?, a% and b% refer to the reference, and L%a*, and b* refer to the test specimen. The signs of the components AL*, Aa*, and Ab* have the following approximate meanings (8): +AL* = lighter -AL* = darker +Aa* = redder (less green) -Aa* = greener (less red) +Ab* = yellow (less blue) -A* = bluer (less yellow) 6.2.6 For judging the direction of the color difference between two colors, it is useful to calculate their CIE 1976 hue angles hab and CIE 1976 chromas C*b as follows: hab = tan~`(b*/a*) C*ab = [(a*)2 + (b*f]Vi Differences in hue angle Ahab between the test specimen and reference can be correlated with differences in their visually perceived hue, except for very dark colors (9). Differences in chroma AC** can similarly be, correlated with differences in visually perceived chroma. 6.2.7 For judging the relative contributions of differences in lightness, chroma, and hue to the total color difference between two colors, it is useful to calculate the CIE 1976 hue difference AH*h between them as follows: AH*h = [(AE*abf - (AL*)2 - (AC**)2]* where AE*b is calculated as in 6.2.1 and C%b is calculated as in 6.2.6; then the equation AEL = [(AL*)2 + (A C*abf + (AHLfl contains terms showing the relative contributions oflightness difference AL*, chroma difference AC*b, and hue difference AH*b to the total color difference AE%b. 6.3 Hunter LH, aH, bH Color Space and Color-Difference Equation (2)--This approximately uniform color space is produced by plotting in rectangular coordinates the quanti ties L/f, alf, bH calculated as follows: ., . L// = 10( 7)Vl aH= 17.5(1.02Z- Y)j( Y)'h bH = 7.0( Y -- 0.847Z)/(7)l/! where X, Y, and Z are tristimulus values for the CIE 1931 standard observer and standard iUuminant C........................ NNO' 3--The subscript L was used to denote Hunter in previous issues of this method. 6.3.1 The total difference AEh between two colors each given in terms of LH, a,,, b,, is calculated as follows: AEh = i(AL,,)2 + + (4iw)f 6.3.2 The magnitude and direction of the color difference are described by considerations similar to those found in 6.2.4 and 6.2.5, respectively. 6.4 Friele-MacAdam-Chickering Color Space and ColorDifference Equation (3,10)--This color space is more nearly perceptually uniform than the CIE 1931 space in terms of the MacAdam chromaticity-difference values (11). It is producedby a linear transformation of CIE 1931 tristimulus values X, Y, Z into tristimulus values P, Q, S as follows: P = 0.724Z + 0.3827 - 0.098Z, Q = -0.48Z + 1.377 + 0.1276Z, 5 = 0.686 Z. Approximate lightness difference ALfmc.2 and chromatic differences AC, ("yellow-blue") and AC3 ("red-green") are calculated a? follows: ALf mc -2 = 0.279KLPAP + QAQ)laD AC, = K,S(PAP + QAQ)/bD2 - fCtAS/b AC3 = K^QAP - PAQ)faD where: a2 = 17.3 x 10~6(.P2 + <22)/[l + 2.TiP2Q2j(PA + Q4)] 6? = 3.098 x 10-4(S2 + 0.2015 72) b = (p2 + q 2T if, = 0.55669 + 0.049434 7 - 0.82575 10~372 + 0.79172 X 10~573 - 0.30087-10-?74 Ki = Q.17548 + Q.027556 7 - 0.57262-10~372 + 0.63893 X 1CTJ 73 - 0.26731 10~774 NQR' 4--The correlations between ALp*,^ and perceived lightness, between AC, and perceived yellowness-blueness, and between AC3 and perceived redness-greenness, are not well established and should not ie used unless confirmed by visual observations. NOS' 5--When K, -- K2= 1, the FMC-1 equations are obtained. 6.4.2 " The total difference AE^c^ between two colors is calculated as follows: .. AE$yCjx -- U.ALf u c ,2)2 + (AC,)2 + (AC3)21'/< 7. Test Specimens 7.1 This method does not cover preparation techniques, Unless otherwise specified or agreed, prepare specimens in accordance with Practice D 3964. 8. Procedure 8.1 Select appropriate geometric conditions for col measurement in accordance with Guide E 179. 8.2 Operate the instrument in accordance with the man ufacturer's instructions. 8.3 Standardize the instrument with a working standard. Restandardize at sufficient intervals to minimize the effects of instrumental drift. 8.4 When a spectrophotometer is used, obtain the reflec tance vdues ofthe reference Specimen and test specimens, n turn, at a sufficient number ofwavelength intervals to per# accurate calculation of CIE tristimulus values. See Method E 308. 8.5 When a reflectance-reading filter colorimeter is used, obtain the reflectance values of-the reference specimen and1 test, specimens, in turn, with each of the filters. 8.6 scale 8.7 stand curret drift, 8.8 surfac locati specii 9. Ca 9.1 ortri; 9.2 and < descri 10. P 10. 10. each 10. refere AH*b 10. ALff, e T: s. (1) " r n 6 ( (. I (2) 1ti (3) (4) C 278 TJ th *Tl O DUP050297461 # D2244 wo colors each follows: 2j'/! 8.6 When a color-scale-reading colorimeter is used, obtain scale values of the reference and test specimens, in turn. 8.7 For any instrument used, remeasure the working standard to determine whether instrumental drift has oc 10.1.4 For FMC-2 color differences, where desired, ap proximate chromatic differences, AC, and AC3, and the lightness difference, ALFMC_2, for each specimen. 10.1.5 For nonuniform specimens, range of color-dif color difference curred during measurement. Compensate for instrumental ference magnitudes obtained for different areas. those found in drift, if observed, or remeasure specimens. 10.1.6 Description or identification of the method of 8.8 Measure at least three portions of each specimen preparing the specimens. iace and Colore is more nearly >ace in terms of lues (11). It surface to obtain an indication of uniformity. Record the location where these measurements were made on the specimen. 10.1.7 Identification of the instrument used, by the man ufacturer's name and model number, and the color-scale system used. 1931 tristimulus S as follows: 9, Calculation 9.1 Calculate color-scale values L*, a*, b*, or LH, aH, bH, or tristimulus values P, Q, S, if not obtained automatically. 9.2 Calculate color differences AE%b, AEH, or AEFMC-2 , and chromatic and their components, if not obtained automatically, as ("red-green") arc described in 6.2, 6.3, or 6.4, respectively. 11. Precision and Bias 11.1 The MCCA Collaborative Reference Program for Color and Color Difference (12) has surveyed the precision of color and color-difference measurements by sending out pairs of painted chips exhibiting small color differences on a quarterly basis for over 10 years. In a typical recent survey (Report No. 45, October, 1983), 118 instruments were involved. Table 1 gives the mean color differences and their iD - Ki&S/b 10. Report standard deviations for the groups of instruments considered separately in the intercomparison, together with the condi 10.1 Report the following information: tions of analysis and measurement. 10.1.1 Total color difference AE%b, AEH, or AEFMC_2, of 11.1.1 Reproducibility--Based on the between-laboratory Q2/(P4 + Q4)l each test specimen from its reference. standard deviations, two color-difference results, obtained by 10.1.2 For CIELAB color differences, L*0, a*0, b*0 for the operators in different laboratories should be considered sus reference, AL*, Aa*, Ab*, and if desired Ahab, AC*b, and pect if they differ by more than the values shown in Table 1. Q^Y2 hH*b for each specimen. 11.2 The precision of color-difference measurements, 10-2YA 0-3y2 T( 7t 4 10.1.3 For Hunter color differences, Lm, aH0, bHi0 and summarized in Table i, was significantly better than the AaH, AbH for each specimen. precision of measured values of color (13,14). id perceived lightnes and between AC3 ai ( red and should noth TABLE 1 Precision of Calculated Color Differences Determined for Various Conditions of Measurement and Analysis Measurement Conditions ,' E No . of Mean Standard Geometry llluminant Observer Equation3 Instruments AE Deviation ations are obtained, tween two colors + (AC>)T 45/0 4570 4570 Sphere0 Sphere0 Sphere0 Sphere0 c 1931 c 1931 1931 c 1931 c 1931 1931 065 1964 Hunter CIELAB CIELAB Hunter CIELAB CIELAB CIELAB 26 0.94 0.04 0.12 17 0.91 0.09 0.27 8 0.95 0.01 0.03 5 0.94 0.10 0.39 34 0.91 0.06 0.17 7 0.92 0.03 0.10 21 0.88 0.02 0.06 . * Maximum acceptable difference. nation techniqui b nunter and CIELAB equations give essentially the same value of AE for the sample pair tested, pare specimens c Specular component included for integrating-sphere measurements. REFERENCES tmditions for col(j "Official Recommendations on Uniform Color Spaces, Color i E 179. Difference Equations, and Psychometric Color Terms," Supple lance with the md ment 2 to CIE Publication No. 15 (E-l.3.1) 1971, Colorimetry (incorporated into CIE Publication No. 15.2 (TC-1.3) 1986, a working stand Colorimetry, 2nd ed.), Bureau Central de la CIE, Paris, 1978. minimize the effej (Available from the U.S. National Committee, CIE, National Institute of Standards and Technology, Gaithersburg, MD) .ed, rnd obtain the refl test specimens `2) ? Hunter, R. S., "Photoelectric Color Difference Meter," Journal of the Optical Society ofAmerica, Vol. 48, 1958, pp. 985-995. Chickering, K. D., "Optimization ofthe MacAdam-Modified 1965 ;th intervals to pen Friele Color Difference Formula," Journal ofthe Optical Society cf s values. See Metl America, Vol. 59, 1967, pp. 537-561. i) Robertson, A. R., "The CIE 1976 Color-Difference Formulae," r colorimeter is uf Color Research and Application, Vol. 2, 1977, pp. 7-11. ference specimen ne filters. (5) Adams, E. Q., "X-Z Planes in the 1931 ICI System of Colorim etry," Journal ofthe Optical Society ofAmerica, Vol. 32, 1942, pp. 168-173. (6) Nickerson, D., and Stultz, K. F., "Color Tolerance Specification," Journal of the Optica! Society of America, Vol. 34, 1944, pp. 550-570. (7) McLaren, K., "The Adams-Nickerson Colour-Difference For mula," Journal of the Society of Dyers and Colourists, Vol. 86,1970, pp. 354-366. (8) McLaren, K., and Taylor, P. F., "The Derivation of Hue- Difference Terms from CIELAB Coordinates," Color Research and Application, Vol. 6, 1981, pp. 75-77. (9) McLaren, K., "CIELAB Hue-Angle Anomalies at Low Tristimulus Ratios," Color Research andApplication, Vol. 5, 1980, pp. 139-143. .. L_. 279 DUP050297462 {10) Chickering, K. D., "FMC Color-Difference Formulas: Clarification Concerning Usage," Journal ofthe Optical Society ofAmerica, Vol. 61, 1971, pp. 118-122. (11) MacAdam, D. L,, "Specification of Small Chromaticity Differ ences," Journal of the Optical Society ofAmerica, Vol. 33, 1943, pp. 18-26. (12) "Manufacturers Council on Color and Appearance Collaborative Reference Program for Color and Color Difference," Collaborative Testing Services, Inc., McLean, VA. (13) Billmeyer, F. W., Jr., and Hemmendinger, H., "Instrumentation for Color Measurement and its Performance," in Golden Jubilee of Colour in the CIE, Society of Dyers and Colourists, Bradford, England, 1981, pp. 98-112. (14) Billmeyer, F. W., Jr., and Alessi, P. J., "Assessment of ColorMeasuring Instruments," Color Research and Application, Vol. 6, 1981, pp. 195-202. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, eitherreapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 280DU P050297463 Designation: D 2246 - 8? Standard Test Method for Finishes on Primed Metallic Substrates for Humidity-Thermal Cycle Cracking1 This standard is issued under the fixed designation D 2246; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method describes conditions for testing an organic coating on a primed metallic substrate for cracking from humidity-thermal cycling or from loss of plasticizer, of both. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 3. Summary of Test Method 3.1 The tendency of an organic coating to develop cracking from humidity-thermal cycling or from loss of plasticizer, or both, is measured by alternate exposure in the humidity cabinet and in the cold box. At the end of the exposure period, the panels are rated for their degree of cracking. 4. Significance and Use 4.1 This test method provides an accelerated means of determining the tendency of an organic coating to fail by cracking when exposed to humidity-thermal cycling. 5. Apparatus 5.1 Humidity Cabinet, of such design and construction as to maintain a relative humidity of 100 % with condensation on the test specimens at all times and a temperature of 100 1F (38 0.5C). 5.2 Cold Box, of such design and construction that a temperature of--10 3F (--23 1.5C) can be maintained. NUV' --Most commercial household freezers are capable of main taining this temperature. 5.3 Rack, as shown in Fig. 1, for supporting test speci mens at an angle of 0 to 30 from the vertical position in 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.27 on Accelerated Testing. Current edition approved May 29, 1987. Published July 1987. Originally Published as D 2246-64 T. Last previous edition D 2246 -65 (I981)el. 2 Annual Book ofASTM Standards, Vol 06.01. such a manner as to prevent contact between them during the test procedure. 5.4 Grid, of thin wires 3 by 8`/2 in. (75 by 215 mm) constituting one hundred and two Vi-in. (13-mm) squares, held in a frame 'h in. wide, with outside dimensions 4 by 9lh in. (100 by 240 mm). 6. Test Specimens 6.1 The test specimens shall be either samples of metallic products, prepared and coated in accordance with the specified production schedule, or coated metallic panels. The recommended panel size is 4 by 12 in. (100 by 305 mm). 7. Preparation of Test Specimens 7.1 The test specimens shall consist of steel meeting the requirements of Methods D 609, cleaned and prepared for coating in accordance with Procedure A of Method D 609. If desired, the metal panels selected for coating with organic coatings may be of any selected composition and may be cleaned and prepared according to commercial practice or by any procedure that is mutually agreed upon. 7.2 After coating, the specimens shall not be cleaned, and they shall be handled only by the edges. 8. Procedure 8.1 Support panels or specimens so that they will be held in a position 0 to 30from the vertical in such a manner as to prevent contact between the panels during the test. 8.2 Place the panels in a humidity cabinet at 100F (38C) and 100 % relative humidity for a period of 24 lA h. Then transfer them to the cold box at --10 3F (-23 1.5C) allowing a maximum of 30 s for the transfer. Leave the panels in the cold box for a period of 20 + 'h h. Remove the panels and allow to remain at room temperature for a period of 4 Va h, during which time rate them. This constitutes one cycle. Run the test for 15 cycles or as mutually agreed upon. During any interruption of the normal cycling, as on weekends, always leave the panels in the cold box. 9. Evaluation of Test Specimens 9.1 Lay the specimen upon a horizontal surface, finish side up, with the framed grid (5.4) placed upon it so that the bottom 8i/2 in. (225 mm) is covered by mesh. (The frame itself excludes the first l/2 in. (13 mm) from edges of the specimen which may have been handled, or which may otherwise not be representative ofthe general area.) Make an evaluation by counting the number of grid squares within which one or more cracks is visible. This number shall constitute the rating. 281 DUP0502 97464 $ 2246 D( 9.2 If the specimen is necessarily smaller than 4 by 12 in. (100 by 305 mm), or is irregular in outline, handle in accordance with 3.4 and 9.1, and assign as the rating the percentage of those grid squares under which the specimen lies, that contain one or more cracks. 9.3 It is recommended that coatings be evaluated by comparison with a coating system known to have acceptable performance. For referee tests this coating system should be included in each test 10. Report 10.1 Report the following information: 10.1.1 Temperature readings within the exposure zone of the humidity cabinet, 10.1.2 Temperature readings vrithin the exposure zone of the cold box, 10.1.3 Method of supporting or suspending panel or specimen during test, 10.114 Exposure period, and 10.1.5 Ratings as described in 9.1 or 9.2. 11. Precision and Bias 11.1 The precision and bias of this test method have not been established. TheAmerican Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Hem mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard ts subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not revised, either reapproved or withdrawn. Your comments ere Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a tab hearing you should make your views known to the ASTM Committee an Standards, 1916 ftece St., Philadelphia, PA 19103. Scope 1.1 This procedures posing coa 100 % rela test specin 1.2 This measuring tests cond specify sp> evaluation NWX' 1-- coatings incl 1.3 Thi. otions, an. address ah the respon. establish t mine the c 2. Referet 2.i a s : D609 N Paint. D 610 1 Paint' D7i4" ; Paint D823 Thic) . Test ' D870 ; ' Usin; D 1193 D 1730 minu D1735 Usinj D2616 Differ 282 1 This prat Related Coat DO 1.27 Accel Current $t published as 2 Annual J 3 Annual i 4 Annual j 5 Annual i DUP050297465 Designation: D 2247 - 87 ire zone of ire zone of , panel or d have not Standard Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity1 This standard is issued under the fixed designation D 2247; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the Department ofDefense. Consult the DoD Index of Specifications and Standardsfor the specific year of issue which has been adopted by the Department ofDefense. j. Scope 1.1 This practice covers the basic principles and operating procedures for testing water resistance of coatings by ex posing coated specimens in an atmosphere maintained at ]0O % relative humidity so that condensation forms on the test specimens. 1.2 This practice is limited to the methods of obtaining, measuring, and controlling the conditions and procedures of tests conducted in 100 % relative humidity. It does not specify specimen preparation, specific test conditions, or evaluation of results. NYZ' 1--Alternative practices for testing the water resistance of coalings include Practices D 870, D 1735, and D 4585. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces2 D714 Test Method for Evaluating Degree of Blistering of Paints2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D870 Practice for Testing Water Resistance of Coatings Using Water Immersion2 D1193 Specification for Reagent Water3 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting4 D1735 Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus2 D2616 Test Method for Evaluation of Visual Color Difference With a Gray Scale5 1 This practice is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee 001.27 Accelerated Testing. Current edition approved Nov. 27, 1987. Published January 1988. Originally Published as D 2247 - 66 T. Last previous edition D 2247 - 86a. 1Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.03 and 11.01. *Annua! Book ofASTM Standards, Vols 02.05 and 06.01. 5 Annual Book ofASTM Standards, Vol [4.02. D3359 Test Method for Measuring Adhesion by Tape Test2 D 3363 Test Method for Film Hardness by Pencil Test2 D4585 Practice for Testing Water Resistance of Coatings Using Controlled Condensation2 -.5. Summary of Practice 3.1 Coated specimens are placed in an enclosed chamber containing a heated, saturated mixture of air and water vapor. The temperature of the chamber is usually maintained at 100F (38C). At 100 % relative humidity (RH), a very small temperature difference between the specimen and the sur rounding vapor causes the formation of condensation on the specimens. The exposure condition is varied by selecting the duration ofthe test. Water permeates the coating at rates that are dependent upon the characteristics of the coating. Any effects such as color change, blistering, loss of adhesion, softening, or embrittlement are observed and reported. 4. Significance and Use 4.1 Water can cause the degradation of coatings, so-knowledge of how a coating resists water is helpful in predicting its service life. Failure in tests at 100 % relative humidity may be caused by a number of factors including a deficiency in the coating itself, contamination of the substrate, or inade quate surface preparation. This practice is therefore useful for evaluating coatings alone or complete coating systems. 4.2 Tests at 100 % relative humidity are used for specifi cation acceptance, quality control, and research and devel opment of coatings and substrate treatments. These tests usually result in a pass or fail determination but the degree of failure may also be measured. A coating system is considered to pass if there is no evidence of water-related failure after a period of time. 4.3 Results obtained from the use of 100 % humidity tests in accordance with this practice should not be represented as being equivalent to a period of exposure to water in the natural environment, until .the degree of quantitative corre lation has been established for the coating or coating system. 4.4 The test chamber can be a small laboratory cabinet or a room large enough to hold an automobile or a truck. Some automobile Manufacturers test completed vehicles in rooms maintained at 100 % relative humidity. Corrosion tests can be conducted, as the condensate dripping off the test articles is not recirculated. 5. Apparatus 5.1 Test Chamber, constructed of corrosion-resistant ma terials with supports for the test specimens. 283 i i DUP05 02 97466 # 0 2247 8. Re 8.1 8.1. 8.1. 0--Angle of k'd, 90 to 125 1--Hinged top. hydraulically operated, or counterbalanced 2--Water seal 3--Constant-level water tank unheated with overflowoutlet and equalize; connection 4--Heater water tank for supplying heat and humidity to cabinet .4? 5--Immersion heater 6--Water temperature limit control 7--'Thermostatic controller for room temperature. Primary limit control for immersion heater (S) 8--Water line 9--Insulation if necessary (see A1.3) 10--Temperature recorder (optional) 1 f--Drain FfG. A1.1 Humidity Cabinet 5.2 Heated Water Tank, within the test chamber, a water supply, and a water level control. 5.3 Thermostatic Control for the water heater with the sensor located adjacent to the specimen holders. 5.4 Thermometer, with sensor located adjacent to the specimen holders. 5.5 Diagrams and details of the apparatus are shown in the Annex. 6. Test Specimens 6.1 This practice does not cover the preparation of test specimens. The substrate composition and surface prepara tion, specimen preparation, and the number of specimens should be agreed upon prior to testing. N[\' 2--Applicable methods for the preparation of test panels and substrates are given in Method D 609 and Practices D 1730. Test Methods D823 cover application techniques for the production of uniform films. 7. Procedure 7.1 Fill the water tank with reagent water conforming to Type TV of Specification D 1193. Tap water may be used, but this will result in the accumulation of residues in the water tank over a period of time. 7.2 Adjust the temperature of the saturated air and water 'apor mixture to 38 1C (100 IT). "* N]^' 3--Due to heat loss to the specimens and the walls of the tamber, the temperature of the water in the tank will .be above the mperature of the air and water vapor mixture. 7.3 Support the specimens approximately 15 from the rtical. Slotted wood supports are suitable for flat speciens. Provide for formation of condensation on the speci mens by spacing them at least 30 mm apart. Space the specimens so they do not touch each otheF, any metallic material, or any material capable ofacting as a wick. Arrange specimens so that condensate from one specimen cannot drip on other specimens. 7.4 Droplets of condensation should be visible on the specimens at all times if the chamber is operating properly. Operate the test continuously with the test chamber closed unless otherwise specified. Short interruptions to inspect or remove specimens are permitted. 7.5 Conclude the test after a specified period of time or after effects from exposure to water are observed. 7.6 Wipe the test specimens dry. Rate specimens for changes in color, blistering, etc. Evaluate specimens no less than 5 min and no more than 10 min after removal from test, as the effects from water exposure can change within a short time. Remove only as many specimens as can be rated within the specified time. N_`' 4--The 0 to 1.0 scale described in ASTM STP SOO6 is preferred for rating. Relevant procedures foe evaluating water effects are described in Test Methods D 610, D 714, D 2616, D 3359, and D 3363. 7.6.1 If possible, rate the specimens again after they have been removed from the test for a recovery period long enough that moisture absorbed within the specimens dries out and the specimens reach moisture equilibrium with room air. A recovery period from 12 to 24 h is generally sufficient. The post-recovery rating allows evaluation of the permanent effects of the exposure as distinct from the transient effects, and is especially important for evaluation of color and gloss. 6 Paint Testing Manual, ASTM STP SOO. ASTM, t972. ! ; i Al. water satura rwater V 1^ >1 1--Ten Z--Fite 3--Ugf 4--The imm 5--Hea 6--Imir, 7--Wai 8--Con 9--Equi 10--FlOO ? Nab' - vaporproc fixture at 284 DUP050297467 g. Report g. l Report the following information: g. 1.1 Sample identification. g. 1.2 Results of the evaluation(s). D 2247 8.1.3 Reference to Practice D 2247. 8.1.4 Hours of test duration. 8.1.5 Test temperature. 8.1.6 Special conditions of test or any deviations in test procedure. Space the ' metallic :. Arrange n cannot e on the properly. >er closed nspect or f time or aens for s no less val from within a be rated is preferred e described 3. they have riod long tens dries ium with generally ion of die from the luation of ANNEX (Mandatory Information) Al. Apparatus A 1.1 The apparatus must be constructed so that heated water vapor is generated at the bottom ofthe chamber. This saturates the air immediately above the water tank with uftter vapor. The saturated mixture of water vapor and air <r. 1--Temperature recorder 2--Fiberglass door with magnetic closers and rubber seal; inward sloping sill 3--Light switch 4--Thermostatic controller for room temperature. Primary limit control for immersion heater (8) 5--Heated water tank for supplying heat and humidity to room 6--Immersion heater 7--Water temperature Omit control 8--Constant level water tank unheated with overflow outlet 8--Equalizer connection 10--Floor drain Mo t s --The chamber shall feature waterproof construction with Insulation and raporproof fixtures on the interior, lighting may be accomplished with a fluorescent toure above Insulating glass sealed in the ceiling. Polyvinyl chloride pipe and flanges shall be used for sleeves through walls. , PIG. A1.2 Walk-in Humidity Chamber temperature rises and then cools below the dew point, causing condensation on the specimens. Al .2 The area of the heated water tank should be limited to no more than 25 % of the floor area of the chamber. The use of a large heated water tank would tend to make the temperature within the chamber uniform, and thus inhibit or prevent the formation of condensate on the specimens. The water temperature will be approximately from 10 to 20F (5 to 10C) above the vapor temperature when the water tank and chamber are properly proportioned. A 1.3 Insulation of the enclosure is not required and can possibly interfere with the formation of condensate by reducing the temperature differential within the chamber. It is difficult to produce condensation with small chambers because the temperature differential is slight. A1.4 Large walk-in chambers may require more than one heated water tank to generate the convective currents needed to cause condensation at all points within the chamber. Circulating fans should be used with caution as their use may reduce the temperature differential and limit condensation. A1.5 In a properly operating chamber, condensation is observed on the specimens or parts when the chamber is opened for inspections. It may be necessary to avoid placing specimens in the lower portion of the chamber as the temperature differentials at the lower levels may be too small to induce condensation. A 1.6 In the event that enough condensation does not occur, or condensation does not form at all the desired points, it is possible to increase condensation by: Al.6.1 Opening the chamber to allow the temperature to drop, Al.6.2 . Turning off the water heater periodically to cause temperature fluctuations, or A 1.6.3 Removing the specimens to allow them to cool down to room temperature. A 1.7 Many variations in the design of the apparatus are possible in the use of this practice. Two typical designs are shown in Figs. AI.l and Ali2. The American Society for Testing and Materials takes no position respecting the validity of any patent rights assailed In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement 0/ such rights, are entirely their own responsibility. , This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Yourcomments are Invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you feet that your comments have not received a fair hearing you should mate1 your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ll 1 '!} 1 i 285 i DUP050297468 Designation: D 2248 - 89 Standard Practice for Detergent Resistance of Organic Finishes1 t the This standard is issued under the fixed designation D 2248; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. sub spe are 1. Scope 1.1 This practice covers the determination ofthe resistance D2244 Test Method for Calculation of Color Differences From Instramentally Measured Color Coordinates2 bat soli use to failure, in an accelerated manner, of organic finishes when immersed in a detergent solution. 3. Significance and Use 1 8' rea, i; 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to 3, 1 Any effects such as color change, blistering, loss of ad- I hesion; softening, or embrittlement are observed and noted. I in ( the address all ofthe safety problems associated with its use. It is ;' the responsibility of the user of this standard to establish appropriate safety and health practices and determine the 4. Apparatus \ 4.1 Container---A corrosion-resistant container equipped sun biotest . applicability ofregulatory limitations prior to use. with the means to control the solution temperature within f reir !the range specified and to control the liquid level at 3/i6 in. rerr 2. Referenced Documents (5 mm). Agitation may be required to maintain temperature | uniformity. | spe> call 2.1 ASTM Standards: D 523 Test Method for Specular Gloss12 D 609 Methods for Preparation of Steel Panels for Testing 4.2 Cover--The container shall be provided with a cover 1 to retard evaporation and to contain the test specimens 1 completely. 1 N this T. Paint, Varnish, Lacquer and Related Products2 D610 Test Method for Evaluating Degree of Rusting on 5. Test Specimens D 61 Painted Steel Surfaces2 D 714 Test Method for Evaluating Degree of Blistering of Paints2 5.1 Unless otherwise specified, the test specimens shall be 4 by 12 in. by 20 gage (100 by 300 by 0.9 mm) in size. The test specimen composition, surface preparation, and number \ i 8 diat spec D823 Test Methods for Producing Films of Uniform of test specimens diall be agreed upon by the purchaser and mui Thickness of Paint, Varnish, and Related Products on the seller. Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 Ncd' 1--Applicable test paneldescription and surface preparation methods are as follows; Methods D 609, Practices D 1730 and D 2092. \ , 9. I 9. ` D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied 6. Coating of Test Specimens s to a Ferrous Base2 6.1 The method ofapplication, film thickness, curing, and D 1400 Test Method for Nondestructive Measurement of conditioning of the test surface shall be agreed upon by the Dry Film Thickness of' Nonconductive Coatings Ap purchaser and the seller. ., |j i plied to a Nonferrous Metal Base2 D 1417 Methods of Testing Rubber Latices--Synthetic3 D1474 Test Methods for Indentation Hardness of Organic Nef' 2--Application and filmthickness measurement methods are given as follows: Test Methods D 823, D 1005, D 1186, and D 1400. . s i s Coatings2 D1654 Method for Evaluation of Painted or Coated 6.2 The backs, cut edges, and those areas containing Specimens Subjected to Corrosive Environments2 identification marks or in contact with the supports, shall be D1730 Practices for Preparation of Aluminum and Alu protected with a suitable coating that is stable under the minum-Alloy Surfaces for Painting4 conditions of test. , [ D2092 Practices for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Paint2 7. Detergent Solution I D 2197 Test Methods for Adhesion of Organic Coatings by 7.1 Composition,' concentration, and temperature of de- j Scrape Adhesion2 tergent solution shall be agreed upon by the purchaser and ; the seller., f 7.2 A typical solid"detergent composition is as follows: f 1 This practice is under the jurisdiction of ASTM Committee D-I on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO l .27 on Accelerated Testing. Tetrasodium pyrophosphate (NauPjO,), anhydrous Parts by Weight ' 53.0 ' % Current edition approved March 31, 1989. Published May 1989. Originally Sodium sulfate (Na2S04), anhydrous published as D 2248 - 64 T. Last previous edition D 2248 - 73 (1982). Sodium metasilicate (Na2Si03), anhydrous 2 Annual Book ofASTM Standards, Vol 06.01. Sodium carbonate (NajCOjJ anhydrous 2 Annual Book ofASTM Standards, Vo!09.01. Sodium salt of a linear alkylarylsulfonate (90 % flake grade) 4 Annual Book ofASTM Standards, Vols 02.05 and 06.01. Total 286 DUP050297469 ices 'ad ted. >ped thin s in. ture over tens 11 be The nber and ation and the . are ung Jibe - the # D 2248 A suggested temperature of the detergent solution is 165 2'F (74 1"C). g_ procedure g,l Immersion--Suspend the test specimens vertically in ^ container so that at least one half of the surface area is ' submerged in the detergent solution. Separate the test specimens so that they are not in contact with any metal and jj-e no closer together than 1 in. (25 mm) at any point in the bath- Replace the detergent solution with fresh detergent solution every 168 h. If successive tests are to be correlated, ^ reference panels coated with a control paint. 3.2 Examination ofSpecimens--When the specimens are jgady for examination, carefully remove, gently wash or dip in clean running water not warmer than the temperature of the detergent solution to remove the detergent from the surface, and then carefully dry by blowing with air or blotting with absorbent paper. During the progress of the test, examine for deterioration of the film immediately. If reimmersion is necessary, do not allow the specimens to rcmain out of the liquid in excess of Vz h, unless otherwise specified. Examine the test coating for the failures specifi cally agreed upon by the purchaser and the seller. Ngh' 3--The following methods of evaluating finish degradation in this method are applicable: Test Methods D523, D7I4, D 1474, and D2197, and Methods D 610, D 1-654, and D 2244. 8.3 Length of Test--The length of test and the interme diate examination periods shall be as designated by the specification covering the organic finish being tested or as mutually agreed upon by the purchaser and the seller. 9. Precision and Bias 9.1 Precision data are based on a round robin in which three finishes applied to two substrates were tested in six laboratories with each laboratory making two runs of five replicates of each-variation. Blister failure was reported by all cooperators using Test Method D714. To simplify the evaluation of blistering data the blister ratings were con verted to single numerical values by the formula Frequency Number x Size -s- 10 = Numerical Value. The Frequency Numbers assigned were as follows: No blistering Very few Few Few medium Medium Medium dense Dense to 9 8 6 S 4 2 By this system, few Size 8 blistering would have a numerical value of 6.4. The adequacy of precision depends upon the purpose of the test and should be determined by die user from the data supplied. 9.1.1 Using these numerical values the standard devia tions for the three finishes were as follows (rounded to nearest-tenth): Finish Within Laboratory 1 0.8 2 0.4 3 1.3 9.1.2 Repeatability: Between-Laboratoty 1.4 0.6 2.6 Finish 1 2 3 9.1.3 Reproducibility: Difference 2.8 1.5 4.5 Finish 1 2 3 Difference 4.9 2.2 9.0 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patera rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are Invited either torrevision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you my attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. f de and /s: /eight w 287 DUP050297470 fit <1 Designation: D 2336 - 87 (Reapproved 1991)e1 Standard Practice for Specifying Properties from Liquid Through Cured State for Coatings Factory Applied to Wood Products1 This standard is issued under the fixed designation D 2336; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon () indicates an editorial change since the last revision or reapprovai. el Nij' --Keywords were added editorially in August 1991. 1. Scope 1.1 This practice summarizes the test methods that may be used to assist in quality control during application and in specifying pigmented coatings that shall be used in factory finishing of wood products. 1.2 This practice is not intended for use by the consumer of coated wood products in specifying such coated wood products. 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user ofthis standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 154 Guide for Testing Varnishes21 D 523 Test Method for Specular Gloss2 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer2 D 869 Test Method for Evaluating Degree of Settling of Paint2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D 1200 Test Method for Viscosity by Ford Viscosity Cup2. D 1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems2 D 1212 Methods for Measurement of Wet Film Thickness of Organic Coatings2 D 1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 D1474 Test Methods for Indentation Hardness of Organic Coatings2 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products2 D1644 Test Methods for Nonvolatile Content of Varnishes2 D1729 Practice for Visual Evaluation of Color Differences of Opaque Materials3 D2196 Test Methods for Rheological Properties of NonNewtonian Materials by Rotational (Brookfield) Vis- # cometer2 D 2197 Test Methods for Adhesion ofOrganic Coatings by Scrape Adhesion2 D 2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates2 D2691 Test Methods for Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products2 D2793 Test Method for Block Resistance of Organic Coatings on Wood Substrates2 D 2801 Test Method for Leveling Characteristics of Paints by Draw-Down Method4 D2805 Test Method for Hiding Power of Paints by Reflectometry2 D 3003 Test Method for Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates2 D 3259 Practice for Infrared Determination of the Tem perature of Applied Coatings on Wood Products During the Cluing Cycle2 D 3278 Test Methods for Flash Point of Liquids by SetaFlash Closed-Cup Apparatus5 D3359 Test . Methods for Measuring Adhesion by Tape Test2 D 3960 Practice for Determining Volatile Organic Content (VOC) of Paints and Related Coatings2 2.2 U.S. Federal Test Method: 14lb/3011 Condition in Container6. 3. Significance and Use' 3.1 Control of the parameters that are measured by the test methods outlined in this practice has been found to be the primary determinant of coating quality and reproduc ibility in the package, during coating application and on the coated product. Accurate measurement is essential if such control is to be achieved. 1 This practice is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcomittee DO 1.52 on Factory-Coated Wood Building Products. Current edition approved Oct 30, 1987. Published December 1987. Originally published as D 2336 - 65 T. Last previous edition D 2336 - 81. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 4 Discontinued; see 1989 Annual Book ofASTM Standards, Vol 06.01. ^Annual Book ofASTM Standards, Vol 06.03. 6 Available from Standardization Documents Order Desk* Bldg. 4 Section D. 700 Robbins Ave., Philadelphia, PA 19111-5094. f \ 4. Chai 4.1 ^ 4.2 S Method Method Both of rather t; torily. 4.3 S Removt well-mi 4.4 C ably dei it. Con Method therer i viscosiri efflux r Rotatio: widely 1 4.4.1 spray, c doubtfu truly in product satisfact 4.4.2 formula either n that fori previoui product: 4.5 F detennii based o particles test doef the pigr disperse remain! pigmen with sai size of batches be said t control adequati 4.6 Vi in accor to-batch is not re 4.7 N mined ir measure film-forr 4.8 V, in accon uniformi where re 4.9 FI with Tes DUPO 502 97471 ;nt of ;rences f Non1) Vismgs by :rences s2 \ent of cts2 trganic Paints its by ocking tes2 TemDuring / SetaTape ntent by the 1 to be roducon the f such l. iction D, D 2336 4. Characteristics in the Package 4.1 Skinning, Settling, and Condition in the Container: 4.2 Settling is determined in accordance with Test Method D869, and by Federal Test Method No. 141b, Method 3011 which also covers condition in the container, goth of these methods are designed for trade sales type paints father than industrial coatings, but could be adapted satisfac torily. 4.3 Skinning can occur in a partially filled container. Remove insoluble skins and perform a skinning test on a well-mixed portion in accordance with Guide D 1541 4.4 Consistency--Consistency of a paint varies consider ably depending upon the type ofinstrument used to measure it. Consistency is determined in accordance with Test Method D 562 and Test Method D 1200. For most coatings therer is not a straight line relationship between Stonner viscosity, a rotational method, and Ford cup viscosity, an efflux method. (The Zahn efflux cup and the Brookfield Rotational Viscometer (Test Methods D 2196) are also used widely by the paint industry.) 4.4.1 Most factory wood finishing is done with airless spray, curtain coating, or roller coating techniques. It is doubtful that any single method of viscosity measurement is truly indicative of the ability of coatings to be applied by production methods or, more especially, to be applied, satisfactorily by curtain coating. 4.4.2 These methods are useful in that once a certain formula has been established, control of the viscosity by either method helps to ensure subsequent reproduction of that formula. In this way, they would be useful in specifying previously qualified coatings for factory finishing of wood products. 4.5 Fineness of Dispersion--The fineness of dispersion determined in accordance with Test Method D 1210, is based on visual observation of a few of the largest size particles remaining in a .coating after dispersion. In itself, the test does not indicate the degree of dispersion of the bulk of the pigment in the coating except that when batches are dispersed in similar equipment the ratio of large particles remaining in the coating to the dispersion of the bulk of the pigment tends to remain constant Therefore, if in an enamel with satisfactory gloss no particles remain that are above a size of 0.5 mil (7 Hegman dispersion), then successive batches of that coating having a similar Hegman rating can be said to have a good enamel grind. Hiding power and color control along with fineness of dispersion control should be adequate to ensure proper dispersion. 4.6 Weight per Gallon--Weight per gallon is determined in accordance with Test Method D 1475 to ensure batch- to-batch and composition product uniformity. This method is not related to the quality of the coatings per se. 4.7 Nonvolatile Content--Non-volatile content is deter mined in accordance with Test Methods D 1644 as another measure of coating uniformity and of the amount of film-forming material provided. 4.8 Volatile Organic Content (VOC)--VOC is determined in accordance with Practice D 3960 both to ensure coating uniformity and to comply with governmental regulation where required. ............ _................ .... 4.9 Flash Point--Flash point is determined in accordance with Test Methods D 3278 as a measure of the degree of flammability or fire hazard of a coating material. 5. Coating Characteristics During and Immediately After Application 5.1 Flow--Flow is a property related to consistency, but it is influenced by other factors such as rate and order of solvent release. Visual observation of the leveling ofa coating film during and after drying and the tendency of the film to sag during application and drying are usually adequate to determine flow. However, Test Method D 2801 may be used if desired. 5.2 Gloss--Specular gloss may be determined in accor dance with Test Method D 523. 5.3 Hiding Power--Hiding power determined in accor dancewith Test Method D 2805 is a measure of the ability of a paint to hide the substrate. It is dependent upon uniform film thickness which is influenced by flow and leveling. 5.4 Wet Film Thickness--The thickness of a wet paint film is determined in accordance with Test Methods D 1212 as a rapid indication that the required amount of coating has been applied. 6. Coating Characteristics During and Immediately After Curmg , 6.1 Curing Temperature--The temperature of a coating film during the curing cycle is an important quality control parameter and should be monitored. Practice D 3259, dis cusses several infrared measuring instruments that can be used for such monitoring. Infrared measuring instruments can be based on the measurement of carefully filtered narrow bands of infrared energy emitted from test surfaces and can be unaffected by surface color or gloss. Thermocouples have been used but are subject to the defects that metals are good heat conductors and do not necessarily absorb heat from infrared radiation at the same rate as the paint film. Better results are obtained with portable pyrometers if they are preheated slightly above the operating temperature. Papers impregnated with wax powders of varying melting points have been suggested also. These tend to absorb infrared energy faster than most wet paint films and, therefore, give higher temperatures than actual. 6.2 Film Thickness--Measurement of film thickness in accordance with Test Methods D 1005, is designed for use on plane rigid surfaces such as metal or glass. It can be adapted to forest products by the simple use of an auxiliary panel of metal or glass placed alongside the wood substrate and coated in the identical way that the wood substrate is coated. Test Methods D 1400 or D 1186 also could be adapted to the forest products industry in a similar manner. This is a simpler but perhaps less accurate method. This adaptation leads to a measurement of application rate rather than to a true measurement offilm thickness of the coating on a wood product because of the possibility of penetration by the coating into the wood product. Test Methods D 2691 gives a method for measuring the actual film thickness present on a wood products substrate. 6.3 Hardness--The measurement of hardness of coating films by means of an indenter, as described in Test Methods D 1474, calls for the measurement of film hardness on smooth, rigid substrates such as glass or metal. There may be some question as to its applicability on films applied to some 289 DUP050297472 D 2336 of the softer forest products substrates. However, ifthe films are thick enough (1.5 mils or greater), it should be applicable on the harder forest products substrate. 6.4 Color Difference--Color difference between a product and the standard can be measured instrumentaUy. Generally, the tolerance is agreed upon by the purchaser and the seller and may also be required if a product specification is involved. Although color instruments are not more sensitive than the eye, and Practice D 1729 may be used for visual evaluation of color differences, color instruments do provide numerical values that can be subsequently compared to later measurements. Test Method D 2244 covers the instrumental determination of small color differences observable in day light illumination between nonfluarescent, nonmetameric, or opaque surfaces such as coated specimens. If metamerism is suspected, visual evaluation should be used to verify the results. 1 6.5 Adhesion--There are no available ASTM test methods directly applicable to measuring adhesion on forest products substrates. It has been found that the available test methods have poor precision even on hard, smooth substrates. They would probably be even less satisfactory on wood substrates. Two methods that might give some indication of adhesion are Test Methods D 2197 and D 3359. 6.6 Blocking--Many coated wood products are immedi ately stacked after curing. Often they are subject to "blocking" or sticking together ifimproperly coated or cured. Test Method D 27937 may be used to detect and quantify the degree of blocking. It may be used as a control test to detect this condition during the coating operation. 7. Keywords 7.1 cured properties; factory application; wood coatings; wood products T Subcommittee'D01.52 is developing a revision to Test Method D3003 to replace Test Method D 2793. The American Society for Testing andMaterials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision atany time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved orwithdrawn. Your comments are invitedeither for revision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. Sco 1.1 extent coalesc thawin 1.2 citions, addra the re approi applic 2. Re 2.1 D5 S 3. Su 3.1 cham -- 15I speck rema: equil: adjus comf origit ; 4. Si 4. j freez | appl i met! ! thest 5. A 5. cont (25 shot I betv 5. I 5. 290^ and \ mine Ci publi DU P050297473 I Designation: D 2337 - 84 {Reapproved 1989) Standard Test Method for Freeze-Thaw Stability of Multicolor Lacquers1 This standard is issued under the fixed designation D 2337; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last ^approval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the ,ent to which multicolor lacquers resist coagulation and coalescence when subjected to freezing and subsequent thawing. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is jjje responsibility of the user of this standard to establish appropriate safety and health practices and determine ike applicability of regulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D 562 Test Method for Consistency of Paints Using the Stormer Viscometer2 3. Summary of Test Method 3.1 Specimens of multicolor lacquers are placed in a chamber maintained at a temperature between -10 and -15"F (-23 and --26C) and allowed to remain 24 h. The specimens are removed from the chamber and allowed to remain at room temperature for 24 h to reach thermal equilibrium. After the specimens are mixed and the viscosity adjusted, they are then sprayed and allowed to dry before comparing with the control standard sprayed from the original specimen. 4. Significance and Use 4.1 Waterborne coatings, when subjected to cycles of freezing and thawing, can undergo detrimental changes in application and performance characteristics. This test method evaluates the ability of multicolor lacquers to resist these changes. 5. Apparatus and Materials 5.1 Cabinet, Room, or Enclosed Space, large enough to contain the specimens to be tested and allowing at least i in. (25 mm) of air space between the sides of adjacent cans. It should be capable of being maintained at a temperature between -10 and -- 15F (--23 and --26Q. 5.2 Stormer Viscometer, with paddle-type rotor. 5.3 Spray Gun, pressure-feed internal-mix type, tip 0.086 in. (2 mm) in diameter with wide-spray nozzle. ' This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct reponsibility of Subcom mittee 1301.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Nov. 14, 1984. Published January 1985. Originally Published as D 2337 - 65 T. Last previous edition D 2337 - 68 <I979){1. 3 Annual Book ofASTM Standards, Vol 06.01. 5.4 White Paper Stock, minimum size 8 by 11 in. (200 by 280 mm). 6. Preparation of Samples 6.1 For all gloss and semigloss multicolor lacquers, pre pare ten 1-qt (1-L) specimens and for flat multicolor lacquers four 1-qt specimens for testing. Mix the sample from which the specimens are filled well by boxing so that it is of a uniform consistency and appearance. After recording the consistency reading as determined with a Stormer viscometer , (in accordance with Test Method D 562 fill all samples in baked varnish-lined containers and apply the lids promptly to prevent evaporation loss). 7. Preparation of Control Standard 7.1 Prepare a control standard by spraying from one of the 1-qt (1-L) specimens of each product to be tested. Use a coated white paper stock and spray on a sheet at least 8 by 11 in. (200 by 280 mm) in size. Adjust the fluid and atomizing pressures to give a spreading rate of 150 to 200 ft2/gal (3.7 to 4.9 m2/L) for complete covering and 200 to 300 ft2/gal (4.9 to 7.35 m2/L) for scatter coat application. 8. Exposure of Samples to Test Conditions 8.1 Place nine specimens of all gloss and semigloss multicolor lacquers and three specimens of all flat multicolor lacquers under test in the chamber that is maintained between --10 and -- 15F (-23 and --26C). Place the specimens on racks in such a manner that they do not touch the walls or bottom of the chamber and so that there is at least 1 in. (25 mm) of air space between adjacent specimens. On each cycle allow all specimens to remain in the chamber for 24 h before removal. Remove from the chamber all specimens of each multicolor lacquer and let them come to thermal equilibrium by allowing them to remain at room temperature (77F (25C)) for 24 h. Mix these specimens to a uniform consistency by boxing. Run a minimum of three specimens and all specimens shall pass the test for multicolor to be acceptable. 9. Examination of Samples and Spray After Test 9.1 Check the consistency of all specimens on the Stormer viscometer after each test cycle and adjust if necessary by adding water to the viscosity of the original before testing. Spray three specimens after each cycle on white paper stock using the same equipment and adjustments of the spray gun that were used to spray the control standard. Allow the sprayed panels to dry thoroughly (16 h) and compare with the control standard in each case for color, particle size, and pattern of the background as well as the accent colors. 291 D UP050297474 D 2337 <f 10. Report 11. Precision 10.1 Report significant change in color, particle size, or 11.1 It is recognized that the seller has no control over the IS:" k' tendency to show coalescence or coagulation when com pared with the control standard. To be considered satisfac tory for freeze-thaw resistance, all gloss and semigloss conditions under which the purchaser will apply multicolor lacquer finishes and, therefore, meaningful estimates of precision cannot be given. In round-robin tests fairly good multicolor lacquers shall show a satisfactory appearance after agreement was obtained by the cooperators as long as the three cycles and all flat multicolor lacquers shall show a same equipment was used to spray the multicolor before and satisfactory appearance after one cycle. after the test The American Society for Testing andMaterials takes noposition respecting the validity ofany patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such pedant rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Commutes on Standards, ISIS Race St., Philadelphia, PA 19103. St [ aU aa \ tht * \ ap f \ ap 2. 3. on sis thf ref i 4. i foi pa m -m,: am mi- pui size iuSi No. 292 DUP050297475 ver the ticolor ites of / good as the 're and Designation: D 2338 - 84 (Reapproved 1989)e1 Standard Test Method for Determining Particle Size of Multicolor Lacquers1 This standard is issued under the fixed designation D 2338; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. ei Nkl' --Editorial changes were made throughout, including the title, in April 1989. j. Scope 1.1 This test method employs photographic reference standards to evaluate the particle size of multicolor lacquers. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Adjuncts: Grain Sizes (5 photos)2 3. Summary of Test Method 3.1 The samples to be tested are mixed by pouring from one container to another until they are uniform in con sistency before spraying on coated white paper stock. After the lacquers are dry they are compared with photographic reference standards to determine the particle size. 4. Significance and Use 4.1 This test method provides a uniform nomenclature for the producer and user in the identification of the various particle sizes used in the manufacture of nitrocellulose-type multicolor lacquers. 1 This test method is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Aug. 31, 1984. Published January 1985. Originally published as D 2338 - 65 T. Last previous edition D 2338 - 68 (1979)e*. 2 Glossy prints ofthe photographic reference standards showing various particle sizes are available at nominal charge from ASTM Headquarters. Request Adjunct No. 12-423380-00. 5. Reference Standards 5.1 The photographic reference standards2 were prepared by photographing actual sprayed panels of multicolor lac quers that were made in the five particle sizes normally used in commercial multicolor lacquers. The standard designa tions are as follows (Figs. 1 (a), (b), (c)): fine, small, medium, large, and extra large, and represent the correct nomencla ture for properly applied multicolor lacquer. 6. Apparatus 6.1 Spray Gun, pressure-feed intemai-mix type, tip 0.086 in. (2.2 mm) in diameter with wide-spray nozzle. 7. Procedure Nmn' --The particle size of multicolor lacquer is dependent upon the spray conditions during the application procedure. In order to get uniform results the exact spray conditions should be agreed upon between the purchaser and the seller. 7.1 Spray the lacquer on a coated white paper panel with the fluid and atomizing pressures adjusted to give a spreading rate of 150 to 200 ft2/gal (3.7 to 4.9 m2/L) for complete covering and 200 to 300 ft2/gal (4.9 to 7.35 m2/L) for scatter coat application. After the sprayed lacquer is thoroughly dry, determine the particle size on the panel by comparing it to the photographic reference standards.2 8. Precision 8.1 This test method entails the use of visual judgment and as such does not readily lend itself to a precision statement. 8.2 In general there has been good agreement between operators in judgment of particle size. 9 Keywords 9.1 particle size; multicolor lacquers; lacquer The American Society for Testing and Matariala takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration af a meeting at fha responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. jr ir t' 293 DUP050297476 f! D 2338 i I Medium Large FIG. 1(b) Particle Size (for other particle sizes, see Figs. 1(a) and 1(c)) Extra large FIG. 1(c) Particle Size (for other particle sizes, see Figs. 1(a) and 1(b)) 294 j. Scop 1.1 1 0.5 % a 1.2 5 safety i respons establis mine th 2. Reft 2.1 DU 3. Sun 3.1 ' by acid acid-di solutio 4. Sigi 4.1 coating This t deterrr paint t 5. Api 5.1 joint. 5.2 joint. 5.3 5.4 5.5 5.6 5.7 6. Ret 6.1 used i that a Comn 1 Thi and Rel mittee E Cun publish* 2 An< DU PO 50297477 Designation: D 2348 - 91 Standard Test Method for Arsenic in Paint1 This standard is issued under the fixed designation D 2348; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearoflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination,of less than 0.5 % arsenic in whole paint. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility-of whoever uses this standard to-consult and establish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water2 ' 3. Summary of Test Method 3.1 The specimen of liquid paint is prepared for analysis by acid-digestion. The arsenic content of a distillate from the add-digested sample is determined by titration with KBr03 solution. 4. Significance and Use 4.1 The permissible level of toxic elements in certain coatings is specified by governmental regulatory agencies. This test method provides a documented procedure for determining low concentrations of arsenic present in whole paint to determine compliance. 5. Apparatus 5.1 Kjeldahl Flask, 800-mL, with standard-taper 24/40 joint. 5.2 Condenser Delivery Tube, with standard-taper 24/40 joint. 5.3 Mechanical Shaker. 5.4 Gas Burner, suitable for heating Kjeldahl flask. 5.5 Glass or Disposable Syringes, 2 mL capacity. 5.6 Erlenmeyer Flasks, 250 and 500 mL capacity. 5.7 Pipets, 10 mL capacity. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.3 Other grades may be used, provided it is ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent grade water conforming to Type II of Specification D 1193, 6.3 Arsenous Oxide, Standard Solution--Dissolve 0.3241 g.of arsenous oxide (As203) in 25 mL of sodium hydroxide (NaOH) solution (100 g/L). Make slightly acid with sulfuric add (H2S04, 1+8), and dilute to 1.0 L with water. 6.4 Hydrazine Sulfate-Potassium Bromide Solution--Dis solve 20 g of hydrazine sulfate (N2H4-H2S04) and 23 g of potassium bromide (KBr) in 200 mL of concentrated hydro chloric acid (HC1, sp gr 1.19) (Precaution--see 7.1) and dilute to 1 L. 6.5 Methyl Orange Indicator Solution--Dissolve 0.1 g in 100 mL water. 6.6 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03) (Precaution--see 7.1). 6.7 Potassium Bromate, Standard Solution--Dissolve 0.18 g of potassium bromate (KBr03) in water and dilute to 1 L with water. Standardize as follows: Transfer 10.0 mL of standard arsenous oxide solution by pipet to a 250-mL flask. Add. 100 mL of water and 25 mL of" HC1 (sp gr 1.19). Heat to 90C and titrate with KBr03 as described in 8.5. Calculate the standardization factor, F, as follows: F= (0.0032410 x 0.7 574)/K where: 0.0032410 = As203 in 10.0 mL of solution, g, 0.7574 = factor converting As203 to As, and V = KBr03 required for the titration, mL. 6.8 Sodium Chloride (Nad). 6.9 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid (H2S04) (Precaution--see 7.1). 7. Hazards 7.1 Handling concentrated acids can be hazardous. Refer to their individual Material Safety Data Sheets (MSDS). 8. Procedure 8.1 Mix the sample until it is homogeneous, preferably on a mechanical shaker. 8.2 Weigh to 1 mg from a glass syringe, 1.0 g of whole paint directly into the 800-mL Kjeldahl flask, being careful 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paints and Paint Material. Current edition approved Oct 15, 1991. Published December 1991". Originally ' published as D 2348 - 65 T. Last previous edition D 2348 - 85. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY and the "United States Pharmacopeia." 295 DUP050297478 # D 2348 not to get any on the sides ofthe flask. Add approximately 10 boiling aids. 8.3 Digest by adding the following: 40 mL of HN03 (allow to stand 20 min) and 25 mL of H2S04 (allow to stand 5 min). Boil; when charring occurs, add HN03 cautiously until the solution becomes clear and begins to reflux within the flask. The flask should be at about a 45 angle while Higwring. Cool, carefully add 150 mL of water, and boil to sulfur trioxide (S03) fumes. 8.4 Add 100 mL of water and a thermometer to an Erlenmeyer flask. After the solution in the Kjeldahl flask has codled, add 25 mL of water, 25 g of NaCl, and 25 mL of the hydrazine sulfate-potassium bromide solution, and connect the distillation tube so that the delivery end is immersed in the receiving water. Quickly heat the Kjeldahl flask over a small, well-protected flame, and distill into the Erlenmeyer flask (Note 1). Adjust the flame so that the temperature of the distillate solution will rise to 80C in 9 to 11 min, and then discontinue distillation by first removing the thermom eter, lifting the distillation tube out of solution slightly and turning the heat off. Nqr' 1--Although it may be necessary to boil the solution, heating is primarily to bring about evolution of hydrogen chloride (HC1) gas, which carries over the arsenic trichloride (AsC13). Absorption ofevolved HCI gas by water causes a rise in temperature which indicates progress of distillation. If distillation proceeds further, or if a larger quantity of H2S04 than specified is used in digestion, sulfur dioxide (S02) will be distilled and titrated as arsenic. 8.5 Titrate the distillate at once with KBrO, soluti, using 3 drops of methyl orange indicator solution. TowaJ the end of the titration add the KBr03 solution very slowj with constant agitation point is reached when to a prevent a local single drop of excess. The the KBr03 end destroys the final tinge of red. Correct the results for th volume of KBr03 used in a blank determination (digest 5! of pure sucrose, using the same reagents and procedure). ` Nop' 2--The blank titration should not exceed 0.7 mL of KBtQ solution. The method is accurate down to variations in the blank, wyj should not exceed 0.1 mL when reagents from the same lot are used,6 9. Calculation 9.1 Calculate the percent of arsenic in the sample & follows: Arsenic, % -- [(V-- 5) x F)/S] x 100 | where: V = KBr03 solution required for the sample, mL, B = KBr03 solution required for the blank, mL, S = sample used, g, and factor as calculated in 6.7. j f [ 1 i 10. Precision and Bias . 10.1 Precision and bias of this test method have not been determined. . 11. Keywords I ! i < 11.1 arsenic; paint j. Scope 1.1 This nature of taining onl 1.2 This problems a user of th health prai limitations 2. Referen 2.1 AS1 D215 y. Paints D233 N D1193 The American Society for Testing ami Materials takes no position respecting the validity at any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ot infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are Invited either lorrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 3. Signif 3.1 Thi: mining qi containing 4. Reagen 4.1 Pur used in al that all re Committf ical Socie grades mt reagent is lessening 4.2 Pw ences to > conformit 4.3 Am 4.4 Ch. 296 J This test and Related mittee DO 1.2 Current e published as 2 Annual, 3 Annual. * Annual. 5 "Reagen ical Soc. Wa the America Joseph Rosir Pharmacope DU P050297479 solution, i. Toward ;ry slowly The end BrOj just ts for the digest 5 g idure). .ofKBrOj lank, which are used. ample as not been Designation: D 2349 - 90 Standard Test Method for Qualitative Determination of Nature of Solvent Composition in Solvent-Reducible Paints1 This standard is issued under the fixed designation D 2349; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the nature of solvent in solvent-reducible house paints con taining only hydrocarbon solvents. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 215 Methods ofChemical Analysis of White Linseed Oil Paints2 D233 Methods of Sampling and Testing Turpentine3 4 D 1193 Specification for Reagent Water* 3. Significance and Use 3.1 This test method provides a procedure for deter mining qualitatively the composition of solvent in paints containing only hydrocarbon solvents. 4. Reagents 4.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 4.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193. 4.3 Antimony Pentachloride (SbCl5). 4.4 Chloroform. 1This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 25, 1990. Published July 1990. Originally published as D 2349 - 65 T. Last previous edition D 2349 - 72 (1984)('. 3 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Bock ofASTM Standards, Vois 06.03 and 11.01. 5 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc. Washington, DC. For suggestions on the testing ofreagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 4.5 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 4.6 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric acid (H2S04). 5. Preparation of Sample 4.1 Mix and prepare the sample in accordance with Methods-D215. 6. Nature of Solvent 6.1 Transfer approximately 150 g of the paint to a 500-mL flask fitted with a 2-hole cork stopper carrying a spray trap connected with a suitable condenser. Through the other hole in the stopper pass an influx tube for steam. (This tube should dip below the surface of the paint.) Heat the flask in an oil or air bath at 100C and pass through it a current of steam; with the steam still passing through, raise the temperature of the bath to 130C. Catch the distillate in a small separatory funnel; continue distillation until 300 mL of water have been obtained. Portions of this water may be drawn from the cock of the separatory funnel from time to time, but care must be taken not to draw out any of the volatile solvent. 6.2 Let the distillate stand until it separates into two layers, then draw off the water and filter the volatile solvent through a dry filter paper into a dry flask. If the solvent is apparently turpentine, examine the distillate in accordance with Color, Odor, Specific Gravity, Refractive Index and Distillation sections of Methods D 233. If the solvent is a mixture of turpentine and petroleum spirits, an approximate determination of the amount of turpentine may be made in accordance with the Polymerization sections of Methods D 233. (It should be noted that turpentine is slightly soluble in water, about 0.3 to 0.4 mL/100 mL of water.) 6.3 To test for benzene, add a few drops of the distillate to a small quantity of a mixture of HN03 (sp gr 1.42) and H2S04 (sp gr 1.84) and heat cautiously. The characteristic odor of nitrobenzene wifi be noted if benzene is present. Nst' 1--Toluene may give a similar odor, 6.4 If the solvent is apparently all petroleum spirits, no further examination is necessary unless further information is desired. 6.5 When the amount of turpentine in the solvent is so small that its presence is questionable, it may be detected by placing 2 drops of the distillate and 2 to 3 mL of chloroform in a dry test tube and adding 1 drop of SbCl5. A slow or slight change in color indicates the absence of turpentine. A rapid change in color to a dark red or purple indicates the possibility of turpentine. The iodine number for turpentine 297 DUPO 502 97480 # D2349 by the Wijs method under these conditions is approximately 340. An iodine number of 20 or over is additional proof of the presence of turpentine and enables calculation of the approximate amount. 7. Keywords 7 I hydrocarbon solveat; solvent composition TheAmerican Society tor Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk cf infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments ere invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. '!1itf * DUP0502 97481 Last ASTM Designation: D 2353 - 83 Standard Test Method for Flow Ratings of Organic Coatings Using the Shell Flow Comparator rhis test method covers the determination of the flow rating, in terms of flow-out characteristics or degree of film nrtthness, of an organic film applied to a flat substrate, jfflfOovrmer,,iy _u_n_dje_r the j;u__ri_s_d__ic__ti_o__nr*o_f__C__o_m_ _m__it_t_e_er\Di-l _o__n Paint and Related Coatings and Materials, this test method was jjjcontinued m 1992. i 299 DUP050297482 Last ASTM Designation: D 2366 - 68 (Reapproved 1980}e1 Standard Test Method for Accelerated Testing of Moisture Blister Resistance of Exterior House Paints on Wood This test method covers only an accelerated evaluation of the resistance to moisture blistering of exterior house paints for use on wood substrates. Formerly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials, this test method was ! discontinued in 1989. <j Refer to Practice D 45 851. II ] Annual Bock ofASTM Standards, Vol 06.01. I r r ib if a1 , * *4 I: i I IL I *$ F' II 'ft > O- C( 300 DUP050297483 Designation: D 2369 - 90 c 2 paints f0r lethod Standard Test Method for Volatile Content of Coatings1 This standard is issued under the fixed designation D 2369; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reappraval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test methodhas been approvedfor use by agencies ofthe Department ofDefense to replace Method 4041.1 ofFederal Test Method Standard No. 141. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. I Scope ll This test method describes a procedure for the deter mination of the weight percent volatile content of solvent ajucible and water-reducible coatings. Test specimens are jjeated at 110 5C for 60 min. Hf0TE i--The coatings used in these round-robin studies represented jj-dried, air-dried oxidizing, and heat-cured baking systems. 1.2 Sixty minutes at 110 5C is a general purpose'test method based on the precision obtained with both solventreducible and water-reducible coatings (see Section 9). These coatings (single package, heat cured) are commonly applied m factories to automobiles, metal containers, flat (coil) metal and large appliances, and many other metal parts. Nuv' 2--Testing at 110 5"C for 20 min was utilized for the (Stablisbment ofthe original test, method in 1965. Precision data are not available and may not have been properly generated at the time. The nine paints tested then were all solvent-reducible. These conditions, 20 oin at 110 5C, are no longer satisfactory for the determination ofthe volatile content of many coatings being tested at the present time. Water-reducible and solvent-reducible coatings were tested in the development ofTest Method D 2369 using 110 5C for 60 min and 20 min for which precision data have been generated. See Appendix X1 for precision statements on the 20-min oven residence time. 1.3 This test method does not cover multi-package coat ings wherein one or more parts may, at ambient conditions, contain liquid coreactants that are volatile until a chemical reaction has occurred with another component of the multipackage coating. Nwx' 3--Committee D-l is running round-robin studies on the volatiles of multicomponent paint systems. The only change in proce dure is to premix the weighed components in the correct proportions and allow the solvent reduced specimens in the aluminum pans to stand at room temperature for 1 h prior to placing them into the oven. Preliminary results with these changes appear to show that this test method is viable for multicomponent systems. 1.4 This test method may not be applicable to all types of coatings such as some printing inks (see Test Method D4713), and other procedures may be substituted with mutual agreement of the producer and user. Nyz' 4--If unusual decomposition or degradation of the specimen occurs during heating, the actual time and temperature used to cure the coating in practice may be substituted for the time and temperature specified in this test method, subject to mutual agreement of the producer and user. 1.5 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility ofthe user ofthis standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. For a specific hazard statement see Note 6. 2. Referenced Documents 2.1 ASTM Standards: D343 Specification for 2-Ethoxyethyl Acetate (95% Grade)2 D 362 Specification for Industrial Grade Toluene3 D1193 Specification for Reagent Water4 D4713 Test Methods for Nonvolatile Content of Printing Inks, Resin Solutions, and Vehicles5 E 145 Specification for Gravity Convection and Forced- Ventilation Ovens6 E 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals7 3. Summary of Test Method 3.1 A designated quantity of coating specimen is weighed into an aluminum foil dish containing 3 mL of an appro priate solvent, dispersed, and heated in an oven at 110 5C for 60 min, The percent volatile is calculated from the loss in weight. 4. Significance and Use 4.1 This test method is the procedure Of choice for determining volatiles in coatings for the purpose of calcu lating the volatile organic content in coatings under specified test conditions. The inverse value, nonvolatile, is used to determine the weight percent solids content. This informa tion is useful to the paint producer and user and to environmental interests for determining the volatiles emitted by coatings. 5. Apparatus 5.1 Aluminum Foil Dish, 58 mm in diameter by 18 mm 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Sept. 12, 1990. Published November 1990. Originally published as D 2369 - 65 T. Last previous edition D 2369 - 87*2, 2 Discontinued; see 1982 Annual Book ofASTM Standards, Part 29. 3 Annual Book ofASTM Standards, Vot 06.03. 4 Annual Book ofASTM Standards; Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vol 06.01. 6 Annual Book ofASTM Standards, Vol 14.02. 7 Annual Book ofASTM Standards, Vol 15.05. 301 DU P05 02 97484 # D 2369 high with a smooth (planar) bottom surface. Precondition the dishes for 30 min in an oven at 110 5C and store in a desiccator prior to use. 5.2 Forced Draft Oven, Type IIA or Type IIB as specified in Specification E 145. 5.3 Syringe, 5-mL, capable of properly dispensing the coating under test at sufficient rate that the specimen can be dissolved in the solvent (see 7.2). 5.4 Test Tube, with new cork stopper. 5.5 Weighing or Dropping Bottle. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.8 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood, to mean Type II of Specification D 1193. 6.3 Toluene, technical grade, Specification D 362. 6.4 2-Ethoxyethyl Acetate, technical grade, Specification D 343. 7. Procedure 7.1 Mix the sample, preferably on a mechanical shaker or roller, until homogeneous. If air bubbles become entrapped, stir by hand until the air has been removed. 7.2 Using an appropriate weighing container (5.3, 5.4, or 5.5, with the syringe preferred for highest precision), weigh to 0.1 mg, by difference, a specimen of 0.30 0.10 g for coatings believed to have a volatile content less than 40 weight % or a specimen of0.50 0.10 g for coatings believed to have a volatile content greater than 40 weight %, into a tared aluminum foil dish (5.5) into which has been added 3 1 mL of suitable solvent (6.2, 6.3, or 6.4). Add the specimen dropwise, shaking (swirling) the dish to disperse the specimen completely in the solvent. If the material forms a lump that cannot be dispersed, discard the specimen and prepare a new one. Similarly prepare a duplicate. N{|' 5--If the specimen cannot be dispersed in the solvents listed (6.2, 6.3, or 6.4) a compatible solvent may be substituted provided it is no less volatile than 2-ethoxyethyl acetate (6.4). B "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY and the "United States Pharmacopeia." 7.3 Heat the aluminum foil dishes containing the dis persed specimens in the forced draft oven (5.2) for 60 min at 110 5C, j N}~' 6: Precaution--la addition to other precautions, provide f adequate ventilation, consistent with accepted laboratory practice, to l prevent solvent vapors from accumulating to a dangerous level. r 7.4 Remove the dishes from the oven, place immediately 1 in a desiccator, cool to ambient temperature, and weigh to | 0.1 mg. I 8. Calculation j 8.1 Calculate the percent volatile matter, V, in the liquid l coating as follows: I V- 100WJ/Six 100] (i) where: Wt -- weight of dish, W2 = weight of dish plus specimen after heating, and S = specimen weight. 8.2 The percent of nonvolatile matter, N, in the coating may be calculated by difference as follows: IV = 100 - V 9. Precision and Bias (2) ! | j 9.1 The precision estimated for tests at 60 min at 110 5C are based on an interlaboratory study9 in which [ joperator in each of 15 laboratories analyzed in duplicate on 2v 1 different days 7 samples of water-based paints and 8 samples of solvent-based paints containing between 35 and 12%. A volatile material. The paints were commercially supplied.. The results were analyzed statistically in accordance with' f Practice E 180. The within-laboratory coefficient of variation- was found to be 0.5 % relative at 213 degrees of freedom and . f the between-laboratories coefficient of variation was 1.7 %' j relative at 198 degrees of freedom. Based on these coeffi- j dents, the following criteria should be used for judging the \ acceptability of results at the 95 % confidence level. i 9.1.1 Repeatability--Two results, each the mean of dupli- cate determinations, obtained by the same operator on \ different days should be considered suspect if they differ by- | more than 1.5 % relative. 9.1.2 Reproducibility--Two results, each the mean of I duplicate determinations, obtained by operators in different | laboratories should be considered suspect if they differ by E more than 4.7 % relative. 1 9.2 Bias--Bias has not been determined. 41 10. Keywords 1 10.1 nonvolatile determination; VOC baking tempera-'1 ture; VOC in paints; volatile determination <| S' ti n n a w C` w si l ------------------- ijj \ 9 Supporting data are available from ASTM Headquarters. Request B%' D01-1026. ;i 302 DUPO 502 97485 mg the dis, or 60 min ai tions, provijj ry practice, tn s level. immediately ad weigh to n the liquid (I) and the coating (2) in at 110 n which 1 plicate on 2 d 8 samples and 72 % y supplied, dance with of variation eedom and was 1.7 % hese coeffiiudging the /el. in of dupliperator on :y differ by mean of l different differ by APPENDIX (Nonmandatory Information) XI. PRECISION STATEMENT FOR 20-MIN OVEN RESIDENCE XI. 1 Oven residence time of 20 min for the paint test specimen at 110 5C was the original procedure for this method. For information purposes, the precision state ments for 20-min residence time are as follows: XI. 1.1 The precision estimates are based on an interlabo^tory study in which 1 operator in each of 15 laboratories jpalyzed in duplicate on 2 different days 7 samples of water-based paints and 8 samples of solvent-based paints containing from 35 to 72 % volatile material. The paints were commercially supplied. The results were analyzed statistically in accordance with Practice E 180. The withinlaboratory coefficient of variation was found to be 1.1.% relative at 193 df and the between-laboratory coefficient of variation was 2.5 % relative at 178 df. Based on these coefficients the following criteria should be used for judging the acceptability of results at the 95 % confidence level. (a) Repeatability--Two results, each the mean of duplicate determinations, obtained by the same operator on different days, should be considered suspect if they differ by more than 2.9 % relative. (b) Reproducibility--Two results, each the mean of dupli cate determinations, obtained by operators in different laboratories, should be considered suspect if they differ by more than 7.1 % relative. TheAmerican Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this atendard are expressly edvised that determination of the validity of any such patent rights, and the risk of infringement of such' rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments witI receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ;' tempera- Request R& 303 DUP050297486 <1 Designation: D 2370 - 82 (Reapproved 1987)62 Standard Test Method for Tensile Properties of Organic Coatings1 6.5.2 Sheet preferably 2 m N' 1--Othi thick palyethyler, fluoropolymer co This standard is issued under the fixed designation D 2370; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This method has been approvedfor use by agencies ofthe Department ofDefense to replace Method 6224.1 ofFederal Test Method Standards No. 141A. Consult the DoD Index ofSpecifications and Standards for the specific year ofissue which has been adopted by the Department ofDefense. 1' NorE-Paragraph 12.1.2 was editorially changed in November 1987. ,2 N' --Keywords were added editorially in July 1991. 7. Hazards 7.1 Mercun vapors are exi mercury can exceed the TL (in a hood) a when handlin Droplets of m pipet connect* 1. Scope 1.1 This method covers the determination of the elonga tion, tensile strength, and stiffness (modulus of elasticity) of organic coatings when tested as free films. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. Specific hazard statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D 882 Test Methods for Tensile Properties of Thin Plastic Sheeting3 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D 3980 Practice for Interlaboratory Testing of Paint and Related Materials2 3. Summary of Method 3.1 Free unsupported films of the materials to be tested are prepared. The tensile properties of the free films are determined by means of a tensile testing apparatus. 4. Significance and Use 4.1 Tensile properties determined by this method are of value in studying the behavior of coatings subjected to environmental stresses, such as those produced by aging and weathering. (See Refs. (1) through (10).)4 4.2 Tensile properties may vary with specimen thickness, method of preparation, gage length, rate of load application. 1 This method is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.23 on Physical Properties of Applied Paint Films, Current edition approved June 25, 1982. Published September 1982. Originally published as D 2370 - 65 T. Last previous edition D 2370 - 68 (1973). 1 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 08.01. 4 Boldface numbers in parentheses refer to the list of references at the end of this standard. tensile tester response, and type of grips used. Consequently, where precise comparative results are desired, these factors must be carefully controlled. r 5. Description of Terms 5.1 tensile strength (nominal)--the load per original unit area at which a specimen fails or yields in a tension (pull) test. 5.2 elongation--the increase in specimen length from the point of initial load application to the point of film rupture in a tension test- 5.3 stress-strain curve--the curve resulting from a plot of tensile load against the distance ofjaw separation (elongation of specimen). 5.4 stiffness (modulus ofelasticity)--the load per unit area required to elongate the film 1 % from the first point in the stress-strain curve where the slope becomes constant. 5.5 gage length--the initial length of the test specimen between the jaws of the tensile tester. 8. Test Spec! 8.1 The tes that is betwee shall vary by length. The le the gage lengt 8.2 Prepan dures: 8.2.1 Dent 8.2.1.1 Ap dental tin foi on which the liquid, which contact with surface by ir coating of th drawdown pi N' 2--U' test coating. In 6. Apparatus 6.1 Equipment for applying films of uniform thickness as described in Test Methods D 823. 6.2 Micrometer Film Thickness Gage as described in Method D 1005. 6.3 Tensile Tester of the constant rate of jaw separation type, equipped with load cells having capacities of 0.2 to 4.4 lb (100 to 2000 g), and equipped with an indicating device such as an electronic constant speed chart recorder, a digital device that displays numerical values, or a printer that records the numerical values.5 6.4 Precision Specimen Cutter having a double blade with a foot to hold the sample in place.6 6.5 Alternative Substrates on which test material can be deposited. 6.5.1 Dental Tin Foil, preferably 1 mil (25 |im) thick.7 5 Suitable tensile testers are supplied by the Instron Engineering Coip., Canton Mass., the Thwing-Albert Instrument Co., 10960 Dutton Rd,, Philadelphia, PA 19154, and the Tillius Olsen Testing Machine Co., P.O. Box 429, Willow Grow, PA 19090-0429. 6 The JDC Precision Cutter manufactured by Thwing-Albert Instrument Co.. 10960 Dutton Rd., Philadelphia, PA 19154, is satisfactory for this purpose. 7 A .satisfactory source is Yates and Bird, Chicago, IL 60610. j 8.2.1.2 Dl and 50 5 mutually ag nesses must thickness, h (50 pm) are 8.2.1.3 V weathering, flat substrat. boiling liqui contact with 8.2.1.4 A ally agreed i period, rent' substrate an specimen et N' 3--P nick-free edgt necessary to c mm) of waste 8 TeflonFEF Pont de Nemou 9 Dry lubricr Chemical Co., I 304 DUP0502 97487 sequently, ;se factors ginal unit iion (pull) i from the m rupture 1 a plot of dongation r unit area >int in the nt. specimen ickness as :ribed in iparation ).2 to 4.4 ag device a digital inter that alade with Lai can be thick.7 orp., Canton* ladclphia, PA billow Grove, itrument Co., urpose. D2370 6.5.2 Sheet of FEP (fluorinated ethylene-propylene),8 preferably 2 mils (50 pm) thick, coated with a dry lubricant.9 N' 1--Other substrates that may be suitable are 10-rail (250-jim) thick polyethylene (7), photographic paper (8), polished steel (9), and juoropolymer coated metal panels. 7, Hazards 7.1 Mercury--Mercury is a toxic metallic liquid. Its vapors are extremely hazardous. Small amounts of spilled tnercury can vaporize sufficiently at room temperature to exceed the TLV of the vapor. Use with adequate ventilation (in a hood) and clean up spills, immediately. Wear gloves tvhen handling mercury. Containers should be kept closed, proplets of mercury can be picked up by using a small glass pipet connected to a suction flask with a rubber hose. g. Test Specimens 8.1 The test specimens shall be free films having a width that is between V2 and 1 in. (13 and 25 mm). No specimen shall vary by more than 2 % in width along its entire length. The length shall be at least 2 in. (50 mm) longer than the gage length selected for the test. 8.2 Prepare the free films by one of the following proce dures: 8.2.1 Dental Tin Foil Substrate: 8.2.1.1 Apply each material to be tested to a strip of dental tin foil. First, mount the foil on a smooth glass plate on which there may be placed a small pool of high-boiling liquid, which may be useful in holding the foil in close contact with the glass. Spread the foil out to a smooth flat surface by means of a rubber squeegee. Apply a uniform coating of the material on the foil by automatic spray or drawdown procedures given in Test Method D 823, N' 2--Use a liquid that is known to have little or no effect on the test coating. In many cases a light mineral oil would be suitable. 8.2.1.2 Dry the applied films at 73.5 3.5F (23 2C) and 50 5 % relative humidity or bake under conditions mutually agreeable to producer and user. Dry film thick nesses must not vary by more than 5 % of the average film thickness. Most films with a thickness of less than 2.0 mils (50 jim) are very difficult to handle. 8.2.1.3 When required for further treatment such as weathering, remount the coated foil on a convenient smooth, flat substrate such as a glass or steel panel. In this case, a high boiling liquid (Note 2) may be used to hold the foil in close contact with the substrate over extended periods of time. 8.2.1.4 Age or expose the coated foil to conditions mutu ally agreed upon. At the end of the specified or agreed upon period, remove the foil-backed film from the glass or metal substrate and cut the specimens to size using the precision specimen cutter. N' 3--A precision specimen cutter must be used to ensure nick-free edges on the specimens. Even with this instrument, it is necessary to cut each specimen independently, allowing at least 'U in. (6 mm) of waste between specimens. 8 Teflon FEP 2-mil film thickness (Card No. 03111, Item. #22499) from E. L du Pont de Nemours & Co., Inc., Wilmington, DE 19898, is satisfactory. 9 Dry lubricant (MS-122 Fluorocarbon Release Agent) from Miller-Stephenson Chemical Co., Danbury, CT 06810, is satisfactory. 8.2.1.5 Place the foil-backed specimen film side up on a pool of mercury to remove the foil by amalgamation. N' 4--Care should be exercised at all times to prevent the high-boiling liquids used in mounting the foil from coming in contact with the test film as these liquids may soften the film. For instance, the foil should be cleaned before amalgamation since any liquid remaining on the back ofthe foil and the test film will float on the bath of mercury. 8.2.1.6 After amalgamation is completed, pick, up an end of the floating film with tweezers, and carefully brush the unsupported film free of mercury and amalgam with a soft camel hair brush. 8.2.2 FEP Sheet Substrate: 8.2.2.1 Apply each material to be tested to a sheet of FEP. First, cover a smooth, flat, polished glass plate with a sheet of FEP. Coat the sheet uniformly with a dry fluorocarbon lubricant and allow to dry for 24 h at standard conditions. Then apply a uniform coating of the test material on the sheet by automatic spray or drawdown procedures given in Method D 823. 8.2.2.2 Dry the applied films at 73.5 3.5F (23 2C) and 50 5 % relative humidity or bake under conditions mutually agreeable to producer and user. Dry film thick nesses must not vary by more than 5 % of the average film thickness. Most films with a thickness of less than 2.0 mils (50 |im) are very difficult to handle. 8.2.2.3 When required for further treatment such as weathering, remount the coated sheet on a convenient smooth, flat substrate such as a glass or steel panel. 8.2.2.4 Age or expose the coated sheet to conditions mutually agreed upon. At the end of the aging or exposure period, remove the sheet-backed film from the glass or metal substrate, and cut the specimens to size using the precision specimen cutter (see Note 3). Carefully strip the coating film from the sheet substrate. 9. Calibration 9.1 Balance, zero, and calibrate the load weighing and recording system of the tensile tester in accordance with methods specified by the manufacturer. 10. Conditioning 10.1 Unless otherwise agreed upon between the producer and the user, condition the test specimens for at least 24 h at 73.5 3.5T (23 2C) and 50 % relative humidity and test in the same environment. 11. Procedure 11.1 Select a mutually agreed upon gage length in the range of 1 in. (25 mm) to 5 in. (125 mm). 11.2 Prepare 10 test specimens for each material to be evaluated. These specimens should not exhibit any nicks or flaws. Measure the thickness of each specimen to 0.1 mil (2.5 Jim) with a micrometer in accordance with Test Methods D 1005, taking five measurements within the gage length area. 11.3 Set the jaw separation of the tensile tester at the gage length selected. Place the test specimen in the grips of the testing machine, taking care to align the long axis of the specimen1 with an imaginary line joining" the points of attachment of the grips to the machine. Tighten the grips evenly and firmly to the degree necessary to minimize 305 DUPO50297488 D 2370 slipping of the specimen during test. N' 5--Mounting is facilitated by the use of air activated jaws. Line-type jaws will minimize slippage and breakage. The application of pressure-sensitive cloth to the ends ofthe film can improve jaw grip. 11.4 Select a mutually agreed upon rate of elongation (strain rate) that is in the range of 5 to 100 %/min. Set the crosshead speed of the tensile tester to provide this rate for the gage length chosen. N' 6--A rate of elongation should be selected that is optimum for testing the types of materials to be evaluated. For relatively brittle films, elongation rates of 5 to 20 % are suggested. For relatively extensible films, elongation rates of 50 to 100 % are suggested, (Refer to Test Methods D 882 for relation of elongation rate to elongation at break). 11.5 Elongate the test specimen until rupture of the film occurs and evaluate the stress-strain curve as follows: 11.5.1 Determine the specimen elongation by measuring the increase in jaw separation from the point of original load application to the point of rupture. 11.5.2 Measure the tensile pull in pounds (kg) required to rupture the film. 11.5.3 If stiffness is desired, determine the tensile pull in pounds (kg) to elongate the film t % from the first point in the stress-strain curve where the slope becomes constant. 11.6 Using the procedures in sections 11.1 through 11.5, run ten test specimens for each material under test 12. Calculations 12.1 For each specimen compute the following: 12.1.1 The elongation E, in percent from the following equation: where: AL = increase in specimen length to break, and L = initial specimen length (gage length). 12.1.2 The tensile strength, T.S., in pounds per square inch, from the equation: T.S. = {Pk )!(TW) where: PK = tensile pull to rupture, lb (kg), T - thickness of test specimen, in. (mm), and W = width of test specimen, in. (mm). 12.1.3 The stiffness (modulus of elasticity), S, from the following equation: 5 = {PE)/{TW) where: PE = pull in pounds (kg) to elongate the film 1 % from the first point in the stress-strain curve where the slope remains constant, T = thickness of test specimen, in. (mm), and W = width of test specimen, in. (mm). 12.2 Examine the uniformity of the tensile strength and elongation results obtained for the ten specimens measured for a material. Choose one of the following procedures f0r discarding spurious values and calculate the mean of the remaining results: 12.2.1 Use the results from those five specimens showing the highest tensile strength in evaluating all three properties discarding those from the remaining five. This is done on the I basis that the expected errors (nicks or flaws in the specimen breaks within thejaw, slippage in thejaw, etc.) would all tend to produce results on the low side. 12.2.2 Discard the values for those specimens where the 1 tensile strength and elongation values are significantly lower than those for most ofthe specimens. Use the test for outliers given in Practice D 3980. 13. Report 13.1 Report the mean values obtained with the test specimens for: 1J. 1.1 Tensile strength, 13.1.2 Elongation, and 13.1.3 Stiffness (modulus of elasticity), if desired. 13.2 Report the conditions of the test 13.2.1 Procedure for preparation of free fiims, | 13.2.2 Rate of elongation in percent per minute, j 13.2.3 Specimen size (length, width, and thickness), 13.2.4 Temperature and relative humidity during test and j treatment, and 1 13.2.5 Aging and treatment given the specimens. r 14. Precision 14.1 An interlaboratory test ofthis method was conducted in which three coatings (representing a brittle film, a film with limited elasticity, and a very elastic film) were tested by five laboratories. The test was conducted with an lnstron ; tensile tester operated at two elongation rates (10 and 100%) : with a specimen gage length of 2 in. (50 mm) and specimen ; thicknesses of 2.5 to 3.5 mils (65 to 90 pm). The between : laboratory coefficients of variation were found to be 30 % for [ percent elongation and 18 % for tensile strength. Based on these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence i level: 14.1.1 Reproducibility--Two results for percent elonga- ; tion obtained by operators in different laboratories should be ; considered suspect if they differ by more than 118 % of their ; mean. Two results for tensile strength obtained by operators ' in different laboratories should be suspect if they differ by j more than 70 % of their mean. 1 15. Keywords 1 15.1 elongation; organic coatings; stiffness; tensile proper- 1 ties; tensile strength 1 REFERENCES (I) Ashton, H. E,, "Flexibility and Its Retention in Clear Coatings Exposed to Weathering," Journal ofCoatings Technology, Vol 51, No. 653, June 1979, pp. 41-52. (2) Ashton, H. E., "Predicting Durability of Clear Finishes for Wood R from Basic Properties," Journal of Coatings Technology,, Vol 52. II No. 663, April 1980, pp. 63-71. | (3) Beardsle; Exterior Vehicle,' 1967, pp (4) Evans, R Moiphol Fiims," Novemb (5) Holswor Jr., "Phj ofPaint (6) Levine, Recent 1 Technoh 306 DUP050297489  ngth and measured dures f0r m of the 5 showing roperties, neon the ipecimen> d all tend vhere the itly lower >r outliers the test 1. ss), g test and 0 2370 (3) Beardsley, Herbert P,, and Kennedy, Richard J., "Performance of Exterior Paints Based on a Vinyl Acetate-Ethylene Emulsion Vehicle,'' Journal ofPaint Technology, Vol 39, No. 505, February 1967, pp. 88-98. (4) Evans, Robert M., and Fogel, Joseph, "Comparison of Tensile and Morphological Properties With Abrasion Resistance of Urethane Films," Journal of Coatings Technology, Vol 49, No. 634, November 1977, pp. 50-60. (5) Holsworth, Richard M., Provder, Theodore, and Ranig, Alexander, Jr., "Physical Characterization of Coatings Upon Aging," Journal ofPaint Technology, Vol 46, No. 596, September 1974, pp. 76-95. (6) Levine, Eli, Lindlaw, William, and Vona, Joseph A., "Some Recent Developments in Water-Based Systems," Journal of Paint Technology, Vol 41, No. 537, October 1969, pp. 531-536. (7) Pierce, Percy E., and Holsworth, Richard M., "The Mechanical Properties and Performance of Wood Primers," Journal of Paint Technology, Vol 38, No. 501, October 1966, pp. 584-590. (8) Shur, E. G., and Rubin, H., "Accelerated Testing of Finishes For Hardboard," Journal of Paint Technology, Vol 41, No. 537, October 1969, pp. 537-550. (9) Schurr, Garmond G., Hay, T. Kirk, and Van Loo, Maurice, "Possibility of Predicting Exterior Durability by Stress/Strain Measurements," Journal of Paint Technology, Vol 38, No. 501, October 1966, pp. 591-599. (10) Yaseen, M., and Ashton H. E., "Effect of Free Film Preparation Method on Organic Coatings," Journal of Coatings Technology, Vol 49, No. 629, June 1977, pp. 50-58. The American Society tor Testing end Materials takes no position respecting the validity ofany patent rights asserted In connection with any item mentioned in this standard. Users ot this standard are expressly advised that determination of the validity ot any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision ot this standard or for additional standards and should be addressed fo ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel thatyour comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. onducted n, a film tested by a Instron id 100 %) specimen : between 30 % for iased on used for ifidence elongalould be o of their operators differ by le proper- s for Wood gy, Vol 52, 307 DU P0502 97490 Designation: D 2371 - 85 (Reapproved 1990)1 Standard Test Method for Pigment Content of Solvent-Reducible Paints1 This standard is issued under the fixed designation D 2371; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. C1 N' --Section 10 was added editorially in May 1990. 1. Scope 90-mL centrifuge tube a 4-oz (120-mL) screw cap bottle with 1.1 This test method covers the procedure for the quanti tative separation of the vehicle from the pigment in solvent- reducible coatings. 1.2 This test method has been proven to be applicable to the following types of paints: white linseed oil outside house vinyl-lined screw cap may be used.3 4.3 Laboratory Oven, vented and capable of maintaining a temperature of 105 2C. 4.4 Syringe, 5-mL. 4.5 Water Bath. paint, white soya and phthalic alkyd enamel, white linseed ophthalic alkyd enamel, red lead primer, zinc chromate primer, flat white inside enamel, white epoxy enamel, white vinyl toluene modified alkyd, and white amino modified baking enamel. It is considered to be applicable to most solvent-reducible paints. 5. Solvents ' 5.1 Ethyl Ether or Petroleum Ether: (Warning--See 6.1). 5.2 Extraction Mixture--Mix 10 volumes of ethyl ether, 6 volumes of benzene or toluene, 4 volumes of methyl alcohol, and 1 volume of acetone (Warning--See 6.2, 6.3, and 6.4). 1.3 This standard does not purport to address all of the 6. Hazards safety problems associated with its use. It is the responsibility ofthe user ofthis standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. Specific precautionary statements are given in Section 6. 6.1 Ethyl Ether and Petroleum Ether--Flammable. Vapor is harmful. May be fatal if inhaled or swallowed. Use only with adequate ventilation. Avoid prolonged contact with skin. Avoid contact with flame, hot surface, or sparks. Do not get in eyes, on skin, or on clothing. Refer to suppliers' 2. Referenced Document Material Safety Data Sheet. 6.2 Acetone--Flammable. Vapor is harmful. May be fatal 2.1 ASTM Standard: if inhaled or swallowed, Use only with adequate ventilation. D2698 Test Method for Determination of the Pigment Avoid prolonged contact with skin. Avoid contact with j Content of Solvent-Reducible Paints by High-Speed flame, hot surface, or sparks. Do not get in eyes, on skin, or Centrifuging2 on clothing. Refer to suppliers' Material Safety Data Sheet. 3. Significance and Use 6.3 Methyl Alcohol--Flammable. May be fatal or cause blindness if swallowed. Cannot be made nonpoisonous. 3.1 This test method is suitable for setting specifications Harmful if inhaled. Keep away from heat, sparks, or open for the pigment content of solvent-reducible paints as well as flame. Avoid breathing vapor. Use only with adequate for monitoring manufacturing quality control. ventilation. Refer to suppliers' Material Safety Data Sheet. 3.2 This test method provides the isolated pigment frac 6.4 Benzene has been declared carcinogenic. tion from solvent-reducible paints that may be used for 6.4.1 Benzene and Toluene--Flammable. Vapors and pigment analysis. liquid are harmful and may be fatal if swallowed. Keep away 4. Apparatus from heat, sparks, or open flame. Keep in a well-closed container. Avoid breathing vapor. Avoid contact with eyes, 4.1 Centrifuge, explosion-proof, capable of developing skin, or clothing. Refer to suppliers' Material Safety Data < 1000 to 2000 g. Sheet. N' 1--The centrifuge should be equipped with a suitable head to take the proper size trunnion cups necessary for use of the 90-mL tubes or 4-oz (120-mL) bottles. A two, four, or six-place head can be used with the bottles and an eight-place head can be used with the tubes. 4.2 Centrifuge Tube, 90-mL, heavy-walled. In place of the 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paint and Paint Materials. Current edition approved May 31, 1985. Published July 1985. Originally published as D 2371 - 65 T. Last previous edition D 2371 - 73 (1979)1. 2 Annua/ Book ofASTM Standards, Voi 06.01. 7. Procedure 7.1 Mix the sample until it is homogeneous, preferably on a mechanical shaker. 7.2 Weigh to 1 mg from a syringe, 5 to 10 g of sample into a tared 90-mL centrifuge tube with a screw-type glass stirring rod (the rod is tared with the centrifuge tube), or a glass bottle as described in 4.2. The weight of the specimen is the \ j ' j 3 Bottles and caps that have been successfully used may be obtained from the Sargent Welch Scientific, 7300 N. Linder Ave., Skokie, 1L 60076 and are designated i as follows: Cat. No. S9185C, 4-oz bottles. I DU PO 502 97491 lottle with aintaining -See 6.1). yl ether, 6 /I alcohol, and 6.4). >le. Vapor Use only itact with parks. Do suppliers' ry be fatal entilation. itact with >n skin, or ita Sheet. 1 or cause joisonous. or open adequate i Sheet. >ors and ;ep away ell-closed with eyes, ifety Data D2371 weight of syringe and paint minus the weight of the syringe aflter transferring the specimen to the tube or bottle. 7.3 Add 60 mL of extraction mixture (5.2) and stir well #ith the glass, screw-type stirring rod, preferably using a power stirrer. Wash the rod clean with a stream of extraction fixture into the tube, and reserve the rod. If the glass bottle jS used, mixing may be accomplished by hand, shaking vigorously, or by use of a mechanical shaker. 7.4 Centrifuge at 1000 to 2000 g (Note 2) until the pigment is clearly separated. A faster speed may cause the pigment to pack too hard for future mixing. (See Test Method D 2698.) N' 2--Calculate the gravity developed by the centrifuge as fol- lows; g= 1.118 x 10_s x rX n2 (1) where: r = rotating radius, mm, and n = rotating speed, r/min. 7.5 Discard the upper layer by decantation. 7.6 Repeat the extraction twice as described in 7.3, 7.4, and 7.5, making certain that the settled pigment is suffi ciently stirred or shaken so that no lumps can be seen sticking to the side of the centrifuge tube or bottle and all pigment can easily be washed from the stirring rod into the tube. It may be necessary to break up the pigment cake before stirring. The bottle and contents may be mixed by tapping at an angle on a cloth pad on a bench top to break up the pigment cake and then shaking vigorously to complete the pigment dispersion in the extraction mixture. 7.7 Make a fourth extraction using ethyl ether or petro leum ether following the same precautions noted in 7.6. Decant the upper layer. Drive off the ether by heating (gently at first to avoid spattering) on a steam bath in a hood away from open flames or sparks. The pigment should be broken up by tapping the tube or bottle on a cloth pad on a bench top. Dry the tube or the bottle at 105 2C for 2 h. 7.8 Cool and weigh the tube (including stirring rod) or bottle, plus pigment. 8. Calculation 8.1 Calculate the percent of pigment, P, as follows: P=[{W,~ W2)jS\xm (2) where: Wi = weight of the tube (including stirring rod) plus pigment, g, W% - weight of the tube (including stirring rod), g, and S = weight of paint sample used, g. N' 3--All pigment obtained using this test method has minute amounts of vehicle adsorbed on the pigment. However, this will not significantly affect the precision of this test method. 9. Precision 9.1 Data are not available to determine the precision of this test method. There are no plans at present to obtain such data. This test method has been in use for several years and is considered acceptable. 10. Keywords 10.1 high speed centrifuging; pigment content; pigment separation; solvent-reducible paint The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or lor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. II you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race Sf,, Philadelphia, PA 19103. ferably on tmple into ass stirring or a glass men is the ined from the are designated 309 DUP050297492 Designation: D 2372 - 85 (Reapproved 1990)-1 Standard Practice for Separation of Vehicle From Solvent-Reducible Paints1 This standard is issued under the fixed designation D 2372; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. f! N' --Section 6 was added and the title was changed editorially in May 1990. : ; 1. Scope 1.1 This practice covers the procedure for the separation of the vehicle from the pigment in solvent-reducible paint. 1.2 In the development of the practice the following material; were tested: white soya and white fish oil isophthalic utkyd semi-gloss enamels, white linseed oil paint, white soy.' and white linseed o-phthalic alkyd enamels. It is considered to be applicable to similar materials. 1.3 This standard does not purport to address the safety problems :ssociated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability cfregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D2371 Test Method for Pigment Content of Solvent- Reducible Paints2 3 D2698 Test Method for Determination of the Pigment Content of Solvent-Reducible Paints by High-Speed Centrifuging2 3. Significance and Use 3.1 Separation of the vehicle from the pigment in solvent- reducible paints is required in order to characterize vehicles by chemical, spectroscopic, or chromatograph techniques. Characterization of vehicles is important since they play a major role in the performance of coatings. 4. Apparatus 4.1 Centrifuge, high-speed, capable of developing in ex. cess of 10 000 g. i N' 1--Calculate the gravity developed by the centrifuge as fot I lows: * g -- 1.118 x 10-6 x ex r? .j where: 1 r -- rotating radius, mm, and n = rotating speed, r/rain. 5. Procedure * N' 2--If the percent of pigment is desired, see Test Method \ D 2371 and Test Method D 2698. ; 5.1 Mix the sample until it is homogeneous, preferably on { a mechanical shaker. 5.2 Centrifuge about 20 mL of the whole paint on a ' high-speed centrifuge in excess of 10 000 g (Note 1 j for 30 min or until separation is completed. If difficulty is encoun tered, add 10 mL ofa suitable solvent (Note 3). Mix with the | vehicle layer in the centrifuge tube and centrifuge as before. j Pour off the supernatant liquid into a bottle and stopper j under nitrogen for further use. i 1. coit oth< 1 ati<adt the api apt 2. toe (5< slu 3. Pr 4. ui 8 at T r 1This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paint and Paint Materials. Current edition approved May 31, 1985. Published July 1985. Originally published as D 2372 - 65 T. Last previous edition D 2372 - 73 (1979)". 3 Annual Book ofASTM Standards, Vol 06.01. N' 3--If quantitative work must be done on the vehicle, the j weight of the paint specimen and of the added solvent must be known. I 6. Keywords 6.1 centrifuge; paint vehicle separation; solvent-reducible i paint j 1 ` t The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk oI infringement of such rights, are entirely their own responsibility. f This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. II 310 DUP050297493 Designation: D 2376 - 84 (Reapproved 1989) Standard Test Method for Slump of Face Glazing and Bedding Compounds on Metal Sash1 This standard is issued under the fixed designation D 2376; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. "tenze Paim matographic >ortant since atings. oping in ex. itrifuge as f0|. Test Method preferably on paint on a >te 1) for 30 y is encounvlix with the je as before, and stopper vehicle, the ;t be known. t-reducible I. Scope j l This test method covers face glazing or bedding ^pounds, or both, used on exterior steel, aluminum, and ^er metal sash. 1,2 This standard may involve hazardous materials, opergierts, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is fa responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. j, Summary of Test Method 2.1 A triangular bead of glazing or bedding compound is tooled into a steel channel and then placed in a 122 4'F (50 2C) oven for 7 h and then visually inspected for slump. 3. Significance and Use 3.1 This test method provides an accelerated means for predicting slump of such glazing compounds. 4. Apparatus 4.1 Number 28 U.S. Gage Steel Channel (smooth, unpainted), 1 in. (25.4 mm) wide, % in. (12.7 mm) deep, and 8 in. (203 mm) in length. The flanges of the channel shall be approximately at right angles with the web of the channel. TTte fillet at the bottom of the channel shall have an internal radius of no more than '/i6 in. (1.6 mm). 4.2 Gravity Convective Oven, having a temperature con trolled at 122 4F (50 2C). 4.3 Putty Knife. 5. Reagent 5.1 Solvent, such as methyl ethyl ketone or ethylene dichloride. 6. Sampling 6.1 Thoroughly mix the entire contents of a full, previ- 1 This test method is under the jurisdiction of ASTM Committee C-24 on Building Seals and Sealants and is the direct responsibility of Subcommittee CX12 on Oil and Resin Base Glazing and Caulking Compounds. Current edition approved Nov. 30, 1984. Published January 1985. Originally Published as D 2376 - 65 T. Last previous edition D 2376 - 74 (1979). (b) Fails test. FIG. 1 Slump Test Diagram ously unopened container on a clean, nonabsorptive surface, and take from this the sample to be tested. 7. Conditioning 7.1 Condition both the channel and the mixed compound (in a closed container) for at least 5 h at 73,4 3.6F (23 2C). 8. Procedure 8.1 Thoroughly clean the channel with solvent. 8.2 Apply a portion of the thoroughly mixed compound to the channel in a triangular shape with a putty knife as illustrated in Fig. 1(a). 8.3 When the channel is so filled, set it in an oven with the flanges horizontal, as shown in Fig. 1(a), with the mass of the material toward the top, and maintain the temperature at 122 4F (50 TC) for 7 h. 9. Report 9.1 The report shall indicate if there was sagging or slumping of the compound at the top towards the bottom, as illustrated in Fig. 1(6). 9.2 Any sagging or slumping from the original configura tion, Fig. 1(a), shall be construed as failure. 10. Precision and Bias 10.1 No statement is made about the precision or bias for measuring slump since the result merely states whether there is conformance to the criteria for success in the procedure. 311 DUP050297494 D 2376 The American Society for Testing and Materials takes no position respecting the validity of any patent rights assertedIn connection with any item mentioned in this standard. Users of this standard are expressly advised that determination ofthe validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This sfantfard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invitedeither for revision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Stamfords, 1916 Race St, Philadelphia, PA 19103. | !. i r i: $i i is t- *I .! \ | [ - i lt ;I 'i | DU P050297495 Designation: D 2454 - 91 Standard Practice for Determining the Effect of Overbaking on Organic Coatings1 This standard is issued under the fixed designation D 2454; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. j. Scope 1.1 This practice covers the determination of the timetemperature effect of overbaking on the physical and chem ical properties of organic coatings. 1.2 This standard does not purport to address all of the safetyproblems associated with its use. It is the responsibility 0f whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D522 Test Method for Mandrel Bend Test of Attached Organic Coatings2 D 523 Test Method for Specular Gloss2 D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1308 Test Method for Effect of Household- Chemicals on Clear and Pigmented Organic Finishes2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 D1540 Practice for Effect of Chemical Agents on Organic Finishes Used in the Transportation Industry2 D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature2 D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials3 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting4 D1731 Practices for Preparation of Hot-Dip Aluminum Surfaces for Painting4 D2092 Practice for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Painting2 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is.the direct responsibility of Subcommittee DO 1.27 on Accelerated Testing. Current edition approved Feb. 22, 1991. Published April 1991. Originally Published as D 2454 - 66 T. Last previous edition D 2454 - 84a. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 14.02. 4 Annual Book ofASTM Standards, Vols 02.05 and 06.01. D 2197 Test Method for Adhesion of Organic Coatings by Scrape Adhesion2 D2201 Test Method for Preparation of Hot-Dipped Nonpassivated Galvanized Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D 2244 Test Method for Calculation of Color Differences From Instmmentally Measured Color Coordinates2 D 2794 Test Method for Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact)2 D3359 Test Methods for Measuring Adhesion by Tape Test2 D 3363 Test Method for Film Hardness by Pencil Test2 E 805 Practice for Identification of Instrumental Methods of Color or Color-Difference, Measurement of Materials3 3. Terminology 3.1 Definition: 3.1.1 overbaking--an exposure of the coating to a moder ately higher temperature or to a longer period of baking, or both, than recommended by the manufacturer of the coating for normal curing. This condition is in contrast to "heat resistance" which is a parameter relating to the service life of a coating. 4. Summary of Practice 4.1 Four panels are prepared and baked at the schedule normally recommended for the coating. Two of the panels are then removed and the remaining two are subjected to an additional overbake in which the time and temperature are mutually agreed upon between the- purchaser and the seller. The sets of panels, after a suitable conditioning interval, are then evaluated for the properties that are compatible with the substrate. Among these are gloss, color, flexibility, adhesion, impact resistance, and resistance to reagents. Note that glass substrates should not be tested for impact, and zinc-coated substrates can influence both flexibility and impact. 5. Significance and Use 5.1 Most coatings are designed for a specific baking time and temperature. For a variety of reasons (line stoppages, rerouting back through ovens, oven overheating, etc.) the prescribed time or temperature, or both, of the bake is often exceeded. This practice has been found to be useful in evaluating the effects of overbakes on coatings. 6. Materials 6.1 Standard Baking-Type Coating mutually agreed upon between the purchaser and the seller. 313 DU P0502 97496 D 2454 7. Hazards 7.1 The flash points of most solvents used in many organic coatings and related products are low enough that adequate ventilation is needed to avoid exceeding 25 % of the lower explosive limits ofthe solvents when test panels are being prepared and baked. As these materials are considered toxic, take care to avoid inhalation of solvent vapor and unnecessary contact of solvent with the skin. 8. Procedure 8.1 Application ofOrganic Coating: 8.1.1 Apply coatings to steel panels prepared in accord ance with Methods D 609. 8.1.2 Apply coatings to zinc-coated surfaces prepared in accordance with Practices D2092, when zinc has been applied by the hot-dip method or by electroplating. 8.1.3 Apply coatings to nonpassivated galvanized steel prepared in accordance with Test Method D 2201, when the zinc is applied by a continuous galvanizing method using an aluminum-bearing zinc. 8.1.4 Apply coatings to aluminum surfaces on all-alu minum materials prepared in accordance with Practices D 1730. 8.1.5 Apply coatings to hot-dip aluminum coated surfaces prepared in accordance with Practices D 1731. 8.1.6 In cases where a primer is used in practice under the topcoat, apply the entire system to the panels. The film thickness of each coat shall be mutually agreed upon between the purchaser and seller, but, in the absence of such agreement, the total thickness shall be 2 0.2 mils (50 5 pm). 8.1.7 In instances where clear coatings are to be tested, they may be applied to aluminum or white carrara glass, one side of which has been polished to a smooth, high-gloss finish. Other selected substrata previously agreed upon between the purchaser and the seller may also be used. In the absence of a specific agreement between the purchaser and the seller in regard to film thickness, apply the coatings by automatic spray. (Refer to Test Methods D 823, Method A) at a dry film thickness of 2 0.2 mils (50 5 pm). Multiple coats may be used to obtain this film thickness where necessary due to the nature of the coating material (Note 1). Manual spray application or the drawdown method with wire-wound draw bars may be used when automatic equip ment is not available. N ' 1--Dry film thickness should be measured in accordance with Test Methods D 1005, V 1186, or D1400, whichever is applicable. The adhesion, flexibility, and color can vary considerably with thickness. 8.2 Baking: 8.2.1 The baking schedule for each coating including primer, topcoat, and primer/topcoat systems shall be mutu ally agreed upon between the purchaser and the seller and shall include the following: 8.2.1.1 Normal Baking Schedule (Time and Temperature) recommended for the development ofoptimum film proper ties, and 8.2.1.2 Overbaking Cycle--This cycle shall be within practical limits in order to simulate conditions that might be encountered in actual production where baking oven or conveyor lines, or both might malfunction temporarily due to mechanical or electrical failure. 8.3 Prepare four panels of each coating or coating system > and bake them at the schedule normally recommended to obtain optimum properties. Conduct the baking of these \ panels in a mechanical recirculating air oven set to 2F ( l'C) of the specified baking temperature. At the end of the > specified time remove two panels from the oven and subject the remaining two to the overbake cycle by: 8.3.1 A continuation of the normal bake but for a previously agreed upon time, for example, 50 or 100% increase in time, or 8.3.2 Resetting the oven temperature to the agreed \ overbake temperature and then continuing the bake for a specified period of time after the overbake temperature has been reached, or removing the panels until the overbake ! temperature is reached and then baking them for the agreed upon time. 'j N' 2--The conditions described in 8.3.2 are not usually reproduc ible between laboratories or different ovens because of variations in the heating characteristics of ovens. 8.3.3 After the sets of panels have been baked according to'the mutually agreed upon baking cycles, place them in a suitable rack and condition for 24 h at 73.5 3.5F (23 2C) and 50 5 % relative humidity (see Test Methods D 1640) prior to testing. 9. Test Methods 9.1 Determine the properties of both sets of panels in accordance with the following ASTM methods: 9.1.1 Gloss--Test Method D 523. 9.1.2 Color--Practice DT'729 (Visual) or Practice E805 (instrumental), or both 9.1.3 Flexibility--Test Method D522 (conical mandrel and cylindrical mandrel). 9.1.3.1 Heat-aged flexibility values should be determined in accordance with a baking cycle that is in agreement between the purchaser and the seller. 9.1.4 Adhesion--Test Methods D 2197 (mechanical) or D 3359 (tape), or both, 9.1.5 Impact Resistance--Test Method D 2794.5 9.1.6 Hardness--Test Method D 3363 (pencil test). 9.1.7 Exposure to Reagents--If this test is desired, the choice ofmaterials to which the coating is to be exposed shall be governed by the ultimate use of the coating and shall be agreed upon between the purchaser and the seller. The general procedure to be followed in this test is given in Test Method D'1308 or Practice D1540. j | ! : j | j 10. Report 10.1 Report the following information: 10.1.1 Substrate employed, including type and thickness, 10.1.2 Type of coating, 10.1.3 Film thickness, including primer, if any, 10.1.4 Normal bake schedule, or schedules, 10.1.5 Overbake cycle, 10.1.6 Test methods employed, and [ \ 10.1.7 Values determined, including the measured changes between the normal and overbake cycles.5 5 It is suggested that impact resistance be determined by use of the Gardner Variable Impact Tester obtainable from the Gardner Laboratory, Inc., Betbesda, MD. 314 DUP050297497 system ided to f these o 2F J of the subject for a 100% agreed e for a ure has terbake agreed jproducns in the :ording :m in a r (23 lethods nels in J E805 tandrel rmined eement cal) or d, the i shall tall be . The n Test ckness, aasured D 2454 The American Society lor Testing and Materials takes noposition respecting the validity olany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement ofsuch rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DU P0502 97498 ^{jlM Designation: D 2485 - 91 Standard Test Methods for Evaluating Coatings For High Temperature Service1 This standard is issued under the fixed designation D 2485; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover the evaluation of the heatresistant properties of coatings designed to protect steel surfaces exposed to elevated temperatures during their ser vice life. Two test methods are described as follows: Method A--Interior Service Coatings Method B--Exterior Service Coatings. 1.2 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsi bility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 5. 2. Referenced Documents 2.1 ASTM Standards: A 36/A 36M Specification for Structural Steel2 A 283/A 283M Specification for Low and Intermediate Tensile Strength Carbon Steel Plates2 A285/A285M Specification for Pressure Vessel Plates, Carbon Steel, Low- and Intermediate-Tensile Strength2 B 117 Test Method of Salt Spray (Fog) Testing3 D522 Test Methods for Mandrel Bend Test of Attached Organic Coatings4 D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products4 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels4 D1014 Test Method for Conducting Exterior Exposure Tests of Paints on Steel4 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base4 D2200 Pictorial Surface Preparation Standards for Painting Steel Surfaces4 G7 Practice for Atmospheric Environmental Exposure Testing of Nonmetallic Materials5 3. Summary of Test Methods 3.1 Panels suitably coated with the material under test are 1 These test methods are under the jurisdiction of ASTM Committee EM on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.27 on Accelerated Testing. Current edition approved May 15, 1991. Published July 1991. Originally published as D 2485 - 66 T. Last previous edition D 2485 - 84. 2 Annual Book ofASTM Standards, Vol 01.04. 3 Annual Book ofASTM Standards, Vols 03.02 and 06.01. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vol 14.02. evaluated under one or both of two test methods depending on the intended usage. 3.1.1 Test Method A, Interior Service Coatings--Coated panels are heated for 24 h in a muffle furnace at a temperature agreed upon between the purchaser and the seller. One panel is plunged into water and the other cooled and then subjected to a bend test. 3.1.2 Test Method B, Exterior Service Coatings--Coated panels are subjected to temperatures that increase in steps from 400 to 800F (205 to 425C). One panel is subjected to salt spray for 24 h, and one is exposed outdoors for 12 months. 3.2 When tests are completed, the panels are examined for evidence of film degradation including rust formation, blis tering, loss of adhesion, dulling, and chalking. 4. Significance and Use 4.1 Some coating systems are developed for use over steel that is exposed to high temperatures during service life. This method provides an accelerated means of determining the performance of these coating systems. Testing of coatings designed for interior service and of coatings designed for exterior (weather-exposed) service is included. 5. Apparatus 5.1 Automatic spray equipment as described in Test Methods D 823 (Method A) or any other suitable method that will give the required uniformity of film and film thickness. 5.2 Muffle furnace capable of maintaining the tempera tures described in 7.2 and 7.3. 5.2.1 Precaution: Due to the high temperatures involved in operating the muffle furnace, extreme caution should be used. 5.3 Salt spray apparatus as described in Method B 117. 6. Panel Preparation 6.1 Type--Panel dimensions shall be established by prior i agreement between the purchaser and the seller. Use panels of lA in. (6.4 mm) hot-rolled steel conforming to Specifica tion A 36/A 36M or Specification A 283/A 283M, or when appropriate, Specification A285/A285M for the water quench test in Test Method A and for all tests under Test Method B. For the bend test in Test Method A, the panels must be thin and soft enough to be bent as described in Test Methods D 552. 6.2 Cleaning--Clean the panels for both test methods iojl accordance with Methods D609, Methods B or D. Then, using a fine silica sand (graded to pass through a No. 4G (425-pm) sieve), blast the panels for Method B to "wbiter metal (removing all mill scale and rust) so that the panels' 316 DUP05 02 97499 lending Coated e at a nd the cooled Coated n steps :cted to for 12 ned for 'n, Wis er steel fe. This ing the oatings led for n Test method id film mpera- volved uld be 117. >y prior panels ecifica r when water er Test panels in Test hods in . Then, No. 40 '"white" panels # D 24^5 comply with grade A SP-5 of Standard D 2200. Other blast media and blast methods are acceptable if agreed upon between the buyer and the seller. Blast-cleaned panels cannot be subjected to the bend test because they are too thick to bend. 6.3 Coatings Applications--Apply the coatings by auto matic spray, Method A of Test Methods D 823, or by any other suitable method that will assure the required unifor mity of film thickness. The number of coats, technique, and cycle for drying between coats of multicoat systems, limits of dry film thickness, and drying time before exposure shall be established by prior agreement between the purchaser and the seller. Determine dry film thickness in accordance with Test Methods D 1186. Allow coatings that air dry at ambient temperature to dry a 168 h at a temperature of 75 5T (24 2.5C) prior to exposing to test conditions. Bake coatings that require heat conversion in accordance with the recom mendation of the supplier. 7. Procedure 7.1 Sampling--When panels have been coated at another location, select at random from different packages two specimens for each method of each type of coating under investigation. 7.2 Test Method A: 7.2.1 Place one panel each of the two types described in 6.1 and 6.2 coated with each paint under test in a muffle furnace maintained at the test temperature mutually agreed upon between the purchaser and the seller, and allow to remain for 24 h. At the end of this time plunge one of the panels immediately into water maintained at 70 5F (21 2.5C). After removing from the water, examine the coating film for evidence of film failure including dulling, blistering, cracking, and loss of adhesion. Allow the second panel to cool at a room temperature of 75 5F (24 2.5C) for 1 h, then rapidly bend double over a '/2-in. (12.7-mm) diameter steel mandrel with coated side uppermost in accordance with Test Methods D 522, Method B. Examine this panel for evidence of film degradation such as cracking and loss of adhesion. 7.3 Test Method B: 7.3.1 Expose duplicate coated panels finished with the materials under test to the elevated temperature test schedule mutually agreed upon between the purchaser and the seller. In the absence of such a specified schedule use the following: 7.3.2 Place the panels in a muffle furnace maintained at 400F (205C) for 8 h, then increase the temperature to 500F (260C) for 16 h. Increase the temperature in 100F (55C) increments, alternating the time periods indicated, to the final temperature maximum previously agreed to be tween the purchaser and the seller. Thus the schedule would be: 400F (205C) for 8 h 500"F (260C) for 16 h 600F (315C) for 8 h 700F (370C) for 16 h 800"F (425'C) for 8 h N' --Many high temperature paints depend upon service condi tions to provide the extreme heat required to cure or sinter their films. If these paints are never exposed to the extreme heat, they may be found to be unsuitable. Consequently, it is good practice to make observations also at temperatures less than the expected service temperatures. 7.3.3 Remove the test panels and make a visual inspection following exposure at each temperature level for evidence of failure, including peeling, cracking, blistering, abnormal discoloration, or loss of adhesion, using ASTM standards where possible. Disregard such failures up to 'A in. (6.4 mm) in from the edges of the test panels. 7.3.4 At the end of the complete exposure, remove the panels from the oven or muffle furnace and allow to air cool at ambient temperature for a minimum period of 1 h. As described in 7.3.3, inspect for evidence of failure due to the high temperature exposure. 7.3.5 If both panels of each pair pass the heat test satisfactorily, use them, respectively, for salt spray (fog) testing and exterior exposure testing. 7.3.5.1 Place one panel of each pair in a salt spray cabinet operated in accordance with the requirements of Method B 117, for a period of 24 h. At the conclusion of the exposure period, examine each panel for rusting or any evidence of corrosive attack. 7.3.5.2 Expose the second panel of each pair on an insulated-type rack, as described in Practice G 7, or as agreed upon between the purchaser and seller, for a period of 12 months. Make a visual inspection after 6 months and after termination of the exposure. The site to conduct the test and the angle of the exposure rack should be agreed upon between the purchaser and the seller and should relate to the end-use application of the coating. 8. Report 8.1 Report the following information: 8.1.1 Description of substrates, substrate preparation, and application conditions used. 8.1.2 Air drying versus baking schedule used. 8.1.3 Details of outdoor exposure when applicable, in cluding: 8.1.3.1 Exposure site, type (insulated rack, black box, open rack, etc.) and angle of exposure, 8.1.3.2 Date of exposure start, 8.1.3.3 Radiation data in terms of kilojoule per square metre or langleys during exposure period, and 8.1.4 Any defects or changes as described under Section 7. 9. Precision 9.1 Four operators in four laboratories tested six materials covering a range of heat-resistant properties and were able to rank products in order of their heat-resisting qualities. Since rankings were of a qualitative nature, no mathematical statement of reproducibility was established. 10. Keywords 10.1 heating tests, paints; resistance, heat; temperature tests, elevated 317 DUP05 02 97500 D 2485 d The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee andmust be reviewed every five years and ifnot revised, either reapproved orwithdrawn. Your comments are invited eithertorrevision ofthis standard or lor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. SCO] 1.1 ' Jeterm caused ! 1.2 itions, gcldres the ret upprop (ipplici 2. Ref 2.1. D4: Ir 3. Sin 3.1 aging, $ ''; V ! ?; iby 0.2 iwasha ! scrub! ! mcdii i-\: | 4. Si] [ 4.1 | near test r diffei ' rente I 4.: i nece; : ; 4-' E tradi p more .? [ Prop. I voiui i taine [ Met! ^j'i | useft " H resul s tom i i | ------ 318 DU P05 0297501 Designation: D 2486 - 89 Standard Test Method for Scrub Resistance of interior Latex Fiat Wall Paints1 This standard is issued under the fixed designation D 2486; the number immediately following the designation radicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (s) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers an accelerated procedure for determining the resistance of latex flat wall paints to erosion caused by scrubbing, 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D4213 Test Method for Wet Abrasion Resistance of Interior Paints2 3. Summary of Test Method 3.1 The test paint is applied to a black plastic panel. After aging, the coated panel is placed, over a '/2-in. by 10-mil (12.7 by 0.25-mm) shim and held in place on a glass plate in a washability machine by means of a gasketed frame. It is then scrubbed with a nylon bristle brush and an abrasive scrub medium until failure occurs over the shim. 4. Significance and Use 4.1 Interior wall paints often become soiled especially near doorways, windows, and in work and play areas. This test method covers determination of the relative resistance of different wall paints to erosion when repeatedly scrubbed to remove the stains during the life of the paint. 4.2 Results developed by use of this test method do not necessarily represent the scrub resistance of aged paint films. 4.3 This test method measures scrub resistance by the traditional scrub-to-failure concept. Test Method D 4213 is a more precise method that measures essentially the same property by a weight-loss technique and reports it as a volumetric film erosion rate. Test Method D 2486 is main tained as an ASTM standard along with the newer Test Method D4213 because it has served the paint industry usefully for many years, its techniques are familiar, and its results are meaningful. To discard it as a standard would be to minimize a great deal of significant past experience. ' This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.42 on Architectural Finishes. Current edition approved March 6, 1989. Published May 1989. Originally Published as D 2486 - 66 T. Last previous edition D 2486 - 79. 2 Annual Book ofASTM Standards, Vol 06.01. 5. Apparatus 5.1 Washability Machine.3 5.1.1 Accessory Apparatus: (Fig. 1). 5.1.1.1 Nylon Bristle Brush, Rubber Mat, and Holder (total weight 454 g). 5.1.1.2 Glass Plate, measured to fit. 5.1.1.3 Shim, 'A-in. by 10-mils (12.7- by 0.25-mm). 5.1.1.4 Gasketed Frame and Clamps. 5.2 Film Caster,4 having 7-mil (0.18-mm) clearance. 6. Reagents and Materials 6.1 Black Plastic Panels.5 6.2 Masking Tape. 6.3 Flannel Cloth, 6.4 Detergentf 6.5 Scrub Medium1 (Note 1), consisting of the following: grams Water, distilled or deionized Hydroxyethyl cellulose8 Ammonium hydroxide, 28 % Drtergent6 Trisodium phosphate, anhydrous Silica9 10 * Acetic acid (glacial) Preservative*15 49.7 ^ 1.0 0.1 2.0 2.0 45.0 0.2B 0.1 ______ _ 100.0 A Adjust to achieve viscosity of 110 to 120 Krebs Units before * Vary to achieve a pH of 9.5 to 10.0. N' 1--When a referee test is made, prepare fresh medium or use standardized scrub medium7 from a previously unopened container that is no more than 1 year old. 6.5.1 Slowly add the hydroxyethyl cellulose to the water while stirring mechanically. Stir until uniform, then continue stirring for an additional 5 min. Then slowly add 3 drops of 3 The Gardner washability machine Model M-J05A and accessary apparatus, available from the Gardner Laboratories, Inc., 5321 Landy Lane, Bethesda, MD 20014, has been found satisfactory for this purpose. Other straight-line wash testers may be adapted to meet the requirements of this test method. 4 The Dow film.caster, available from the Gardner Laboratories, Inc., has been found satisfactory for this purpose. 5 Lcncta P-121-10N dull black plastic panels 6 'h by 17 in. by 10 mils (165 by 432 by 0.25 mm) in size (production tolerance: 1 mil), obtainable from the Leneta Co., P.O. Box 576, Ho-Ho-Kus, NJ, are suitable for the purpose. 4 Octyl phenoxy polyethoxy ethanol has been found satisfactory. Triton X-100 obtainable from Rohm & Haas Co.. Independence Sq., Philadelphia, PA, is representative of this product. 7 Laboratory standardized scrub medium is available from the Leneta Co. Cellosize QP-4400, obtainable from Union Carbide Corp., Chemicals Div., 270 Park Ave., New York, NY, has been found satisfactory for this purpose, 9 Silica No. 22, obtainable from Whittaker, Clark, & Daniels, Inc., 100 Church St, New York, NY 10007, has been found satisfactory for this purpose. 10 1,3.5-triethyl hexahydro-sym-triazine (Vancide TH) obtainable from R. T. Vanderbilt Co., 230 Park Ave., New York, NY 10017, has been found satisfactory. 319 DUP050297502 D 2486 28 % ammonium hydroxide while mixing, and continue mixing until solution turns clear. In the order given, add the other ingredients separately, employing mechanical stirring. Be sure that each item is uniformly dispersed before adding the next one. The addition of the silica should take about 5 min to ensure uniform dispersion. Finally, add the preserva tive and adjust the pH with glacial acetic acid. 7. Preparation of Apparatus 7.1 Washability Machine--The washability machine should be leveled before use and operated at 37 1 counts per minute. Before each test check the tightness ofthe motor belt or chain drive, alignment of the pulleys and cables in both horizontal and vertical planes, and tautness ofthe cable. 7.2 Brush--The bristles, if new, must be leveled before use to permit uniform wear on the paint surface. Leveling is accomplished by running the brush over 100 or 120-mesh aluminum oxide close grain sandpaper or emery cloth attached lengthwise on the glass plate in the washing machine. The total number of cycles required will vary from 1000 to 5000. Additional weight, up to 454 g, may be used to expedite the procedure. Change the sandpaper or emery cloth if it becomes clogged. Tape down the edges if any tearing is observed. Replace brush when bristles have worn to extend less than 5/s in. (16 mm) from block. 7.3 Brush Holder--Screws on the brush holder shall be removed and not used. Instead, insert a [/s-in. (3.2-mm) thick rubber mat in the holder above the brush block. When in operation, this mat allows the brush to ride evenly on the paint surface without tilting (Fig. 1). The brush must fit loosely in the holder. 8. Procedure 8.1 Clean the top of the glass plate (or preferably suction plate) and both sides of the black plastic panel to be sure they are free of specks. Place the black panel on the plate and tape one end to the plate. Smooth the panel along the plate by rubbing with flannel, creating static electricity which im proves adhesion to the plate. 8.2 Stir the test paint thoroughly and strain to remove all skins and particles. Draw down the paint on the panel using the 7.0-mil (0.18-mm) side of the film caster, starting from the taped end of the panel. The time for application should be fairly slow--3 to 4 s from end to end--to prevent formation of pinholes or holidays in the film. Air dry in a horizontal position for 7 days in an open room kept at 73.5 3.5F (23 2C) and 50 5 % relative humidity. 8.3 Clean the plate and set it in the pan of the washability machine. Be sure that the shim is smooth and free of burrs and placed across the center of the plate. Wipe the test panel carefully and place it on top of the shimmed plate with the painted side up. Be sure that there are no defects in the film above the shim and that the test area is level. Prewet the gasket of the frame and wipe it dry before use. Place the frame over one half of the drawdown, being sure that the entire gasket is on the painted surface. (The other halfcan be used for a second test if desired.) Clamp the gasket in place. The clamps should be tight enough to ensure close contact, but not tight enough to cause warping of the panei. 8.4 Soak the brush in a 1 % solution of detergent6 FIG. 1 Accessory Apparatus for Scrub Test overnight. Remove the brush and shake it vigorously to remove any excess. Mount the brush in the holder being sure that the mat is in place above the brush block and that the brush is always in the same position. (Mark both brush and holder beforehand.) Stir the scrub medium and spread 10 g evenly on the brush bristles. Place the brush at one end ofthe path and attach the guide cables. Wet the panel with 5 mL of reagent water in the path of the brush. 8.5 Set the cycle counter at zero. Start the test. After each 400 cycles before failure remove the brush (do not rinse); add 10 g of stirred scrub medium; replace the brush, being sure that brush and holder are in the same position with relation to each other and in the machine. Place 5 mL of water on the path before continuing. 8.6 Record the number of cycles to remove the paint film fully in one continuous line across the '/2-in. (12.7-mm). width of the shim. Stop the machine and wipe off the area to determine the end point 8.7 Make three drawdowns of each specimen. Test two and average them if they are within 25 % repeatability. If they are not, test a third and average the three, unless one of the results is obviously discrepant, in which case it should be discarded. According to the 90 % confidence limits specified herein, the running of a third test will be required, on the average, only one out of ten times for normal results. 1 i \ f l [ f \ ' ' i [ 320 DUP050297503 D 2486 p, Report 9.1 Report the mean number of cycles to failure (see taction 10). 9.2 Outline any deviations from standard procedure. jO. precision 10.1 The following criteria should be used for judging the acceptability of results of scrub resistance tests at a 90 % confidence level. 10.1.1 Repeatability--Duplicate results by a single oper ator should be considered suspect if they differ by more than 25 % of their mean value. 10.1.2 Reproducibility--Two results (each the mean of duplicate measurements) obtained by operators in different laboratories should be considered suspect if they differ by more than 50 % of their mean. 11. Keywords 11.1 Scrub resistance; abrasion resistance The American Society for Testing andMaterials takes no position respecting the validity of any patentrights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that'determination of the validity of any such patent rights, and the risk of Infringement of Such rights, are entirely their own responsibility. This standard isstiblact to revision at any time by the responsible technical committee andmust be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invitedeither forrevision, of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting at the responsible technical committee, which you may attend. If you feel that your comments heve not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. it usly to ng sure hat the sh and d 10 g ofthe mL of reach ;); add ng sure elation on the nt film 7-ram) area to ist two ility. If one of Duld be lecified on the 321 DUP050297504 1 Designation: D 2571 - 89 <! Standard Guide for Testing Wood Furniture Lacquers1 This standard is issued under the fixed designation D 2571; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This Guide covers the evaluation of gloss or flatted, " unpigmented lacquers designed for use on wood substrates. This Guide is to be used in conjunction with Test Methods D333. Also included are several methods.of special rele vance to the application of lacquer on wood* The sdection of the tests to be used for any given product or system must be governed by experience and by the requirements agreed upon by the producer and user. 1.2 The tests on films apply to those films applied in sufficient quantity to form a continuous film. It is recom mended that reports include the thickness of the film under test. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)^ D 333 Test Methods for Clear and Pigmented Lacquers3 D 1211 Test Method for Temperature-Change Resistance ofClear Nitrocellulose Lacquer Films Applied to Wood3 D1308 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes3 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale)4 D2091 Test Method for Print Resistance of Lacquers3 D2199 Method for Measurement of Plasticizer Migration from Vinyl Fabrics to Lacquers3 D3359 Test Methods for Measuring Adhesion by Tape Test3 D 3459 Test Method for Humid-Dry Cycling for Coatings on Wood and Wood Products3 G23 Practice for Operating Light-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Expo sure of Nonmetallic Materials5 1 This Guide is under the jurisdiction of ASTM Committee D-l on Faint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.5S on Factory-Applied Coatings on Performed Products. Current edition approved March 25, 1988. Published September 1988. Origi nally published as D 2571 -67. Last previous edition D2571 -81(1987). 2 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vois 06.01,06.02 and 06.03. 5 Annual Book ofASTM Standards. Vols 14.02 and 06.03. 3. Significance and Use 3.1 This Guide is intended to compile as well as provide screening tests in evaluating wood furniture coatings both high gloss and flatted type, as used by the furniture industry. 3.2 Each wood finishing system may vary from a simple two-step operation to a complex operation consisting of as many as 15 steps. 3.3 The substrate is a complex and varied substrate that does absorb moisture from the surrounding environment. Variation in the moisture content of the wood before and after coating and during the testing affects the test results. Grease, dirt and foreign matter also affect the test results. 3.4 Results from these various tests are not necessarily useful in evaluating performance of all different types of furniture finishing systems. 4. Test Panels and Panel Preparation I i4.1 Test panels should be regular production finish panels. 4.2 If regular production finish panels are not available, 'f I the producer and the user should agree on the substrate to he used and on the complete finishing system. 5. Nonvolatile Matter 5.1 Test for nonvolatile matter in accordance with Test ; {i Methods D 333. i1 6. Self-Lifting Properties 6.1 Apply a second coat after the first top-coat has been applied and air dried for 1,6, and 24 h. Report any tendency of self-lifting. V 7. Color 7.1 Test color of the liquid lacquer in accordance with Test Method D 1544. 8. Rubbing Properties 8.1 In the absence of a specified procedure, air dry the lacquer 18 h, sand with No. 320 W/D sandpaper wetted with mineral spirits, and then rub with 3-F pumice and paraffin oil (white mineral oil, U.S.P. heavy, or other suitable robbing compound). 8.2 Examine the rubbed surface immediately and after 24 h, or the time agreed upon by the producer and the user, in a (i <: d B tl 5 a tl c< d c< si 322 DUP0502 97505 provide js both dustry, simple g of as ite that nment. re and results. ults. jssarily 'pes of finish iilable, etobe h Test been dency e with # D2571 Godard atmosphere, for example, 73.5 3.5F (23 2C) 50 % relative humidity, and report any difference in appearance. ^ print Test 9.1 Test for resistance to imprinting in accordance with TeSt Method D 2091. j0. Cold Check Test 10.1 Test for resistance to checking and cracking in accordance with Test Method D 1211 on a substrate agreed upon by the producer and the user. Report any difference in appearance. 11. Resistance to Oils, Greases, Cosmetics, and Other Household Chemicals (1.1 Test for resistance to the agents in 11.2 to 11.5. For other household chemicals test in accordance with Test Method D1308. 11.2 Cosmetic Stain--Apply to the finished surface .* heavy smear of lipstick of indelible type and place the panel in a 125F (50C) oven overnight. Remove the lipstick with mineral spirits meeting the requirements of Specification D235, and evaluate. 11.3 Alcohol Resistance--Place 0.5 mL of 50 % ethanol (by weight) in water on the lacquer film and trap with a 2-in. (50-mm) watch glass. Pure, undiluted ethyl alcohol or denatured alcohol conforming to Formula 2-B of the U.S. Bureau of Internal Revenue aire considered equivalent for this test One hundred proof vodka may be used in place of 50 % ethanol. After at least 6 h, remove the watch glass and allow the alcohol to evaporate. Report whitening or spotting that cannot be removed with light polishing using a dry, cotton pad. 11.4 Boiling Water Resistance--Pour 25 mL of boiling distilled or deionized water on the leveled panel and allow to cool to room temperature. Dry and examine. Report graying, spotting, softening, or other film deterioration. 11.5 Coffee Stain Resistance--Prepare coffee by each of the following methods: 11.5.1 Dissolve 1 teaspoon (5 cm3) of instant coffee, 1 teaspoon of sugar, and 1 teaspoon of powdered cream substitute in 8 fl oz (240 mL) of at least 180F distilled or deionized water. 11.5.2 Dissolve 1 teaspoon (5 cm3) of instant coffee and sufficient synthetic sweetener (dry or liquid) to supply 5 mg of saccharin in 8 fl oz (240 mL) of at least 180"F distilled or deionized water. 11.5.3 Place 1 mL of each type of hot coffee on the panel and cover with 2-in. (50-mm) watch glasses. After 2 h, remove the watch glasses, and allow to evaporate. Wash the panel with a rag moistened with water. Report how readily the residue is removed. 12. Light Exposure 12.1 Test for the effect of light exposure in accordance with all methods exeept 1, 2, and 3 of Practice G 23, but operated without water spray. Report method used and results. 13. Tape Marring 13.1 Press a strip of cellophane tape, on the test panel, rolling it down with a 70 to 80 durometer hardness rubber roller. Allow the tape to remain on the panel for 30 min. Slowly remove the tape. After 30 min recovery, report any visible marring. 14. Tape Adhesion 14.1 Test for tape adhesion in accordance with Test Methods D 3359. 15. Resistance to Plasticizer Migration 15.1 Test and rate plasticizer migration in accordance with Test Method D 2199. 16. Accelerating Aging by Humid-Dry Cycling 16.1 Evaluate and report the accelerated aging in accord ance with Test Method D 3459. The American Society for Testing end Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity ot any such patent lights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time try the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invitedeither forrevision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive, careful consideration at a meeting of the responsible technical committee, which you may attend, If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Pace St., Philadelphia, PA 19103. try the :d with araffin ubbing fter 24 er, in a 323 DUP050297506 \ Designation: D 2574 - 86 Standard Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms1 This standard is issued under the fixed designation D 2574; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 'I r \ ij : j| 1 1. Scope 1.1 This test method covers the determination of the, resistance of emulsion paints against attack in the container by microorganisms. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. * 2. Significance and Use 2.1 Spoilage of paint in the container can result in putrefaction, lowered pH, gas formation, and decrease in viscosity. This test method provides a standard procedure for the evaluation of the resistance of emulsion paints to microbial deterioration. The results should enable: (1). the paint manufacturer to select an effective preservative and (2) the supplier of preservatives to evaluate the performance in emulsion paints of competitive and developmental preserva tives. 2.2 This test method should preferably be used by persons who have had basic microbiological training. 3. Apparatus 3.1 Refrigerator, maintained at 10 to 13C. 3.2 Balance, accurate to 0.1 g. 3.3 Swabs, sterile cotton. 3.4 Screwcap Borosilicate Test Tubes, 125 by 15-mm. 3.5 Borosilicate Flasks, 1-L. 3.6 Screwcap Bottles, 150-mL. 3.7 Autoclave, capable of producing 15 psi (103 kPa) of steam pressure at 120C and maintaining it for a minimum of 15 min. An autoclave is not necessary if prepared agar slants are used. 4. Materials 4.1 Culture ofPseudomonas aeruginosa.2 4.2 1 U.S. qt (945 mL) ofPaint Under Test. 4.3 1 U.S. qt (945 mL) of paint identical to 4.2, but containing no microbiocide. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.28 on Biodeteriomtion. Current edition approved May 30, 1986. Published July 1986. Originally published as D 2574 - 67 T. Last previous edition D 2574 - 73 (1980). 2 Suitable culture may be obtained from the American Type Culture Collection, Washington, DC. 4.4 Dehydrated Tryptone-Glucose Extract Agarf 4.5 BeefExtract.4-5 4.6 Tryptone.4'5 4.7 Glucose.4 5 5. Preparation of Materials Nora--Observe conventional microbiological techniques in__ ,,,,s. these tests. Handle all materials so as to avoid contamination from the air, fingers, or work surfaces. i 5.1 Preparation of Tryptone-Glucose Extract Agar Slants:1! 5.1.1' Add 12 g of tryptone-glucose extract agar to 500 mEf! of cold distilled water in a 1-L flask. Heat to boiling wifif frequent agitation to dissolve the medium completely. j 5.1.2 Distribute 10 mL of the dissolved medium into each J of 50 test tubes. 5.1.3 Autoclave tubes (with caps loose) for 15 min at 15 psi (103 kPa) and a temperature of 120C. J_ 5.1.4 Upon removal from the autoclave, tighten caps ancf place the tubes at an approximate 30* angle position to cool^f making a slope about 2 in. (50 mm) long. ;!i 5.1.5 Store agar slants in a refrigerator at 10 to 13C unfits needed. '!,f* J5.2 Preparation of Tryptone-Glucose Extract Broth: 1 5.2.1 Add 1.5 g of beef extract, 2.5 g of tryptone, and 0.5 g of glucose to 500 mL of cold distilled water in a 1000-mffi flask. Heat to boiling to dissolve the medium completely. 5.2.2 Distribute 10 mL of the dissolved medium into eacffl of 50 test tubes. | 5.2.3 Autoclave tubes (with caps loose) for 15 min at 15? . psi (103 kPa) and a temperature of 120*C. | 5.2.4 Upon removal from the autoclave, allow the tubes| to cool to room temperature, tighten the caps, and store until;! needed. - fj 5.3 Inoculation of Tryptone-Glucose Extract Broth WithH Pseudomonas Aeruginosa: J 5.3.1 To an agar culture of Pseudomonas aeruginosa, addfj 3 mL of the tryptone-glucose extract broth prepared in 5.2^ Using a sterile cotton swab, remove bacterial growth from^ the surface of the agar and mix with the broth. 3 Tubed tryptone-glucose extract agar slants available from Difco Laboratories,-; Inc., Detroit, MI 48201, Baltimore Biological Laboratories, Baltimore, MD 2121' or equivalent are suitable for use by those who do not have the necessary; equipment for preparation of their own media. * Available from Difco Laboratories, Inc., Detroit, MI 48201, Ball Biological Laboratories, Baltimore, MD 21218, or equivalent. 5 Tryptone-glucose extract broth may be prepared by dissolving a commi produced tablet in water. Suitable tablets may be obtained from Consol Laboratories, Chicago Heights, IL. 324 DU P050297507 aking m the ants: ) mL with each it 15 and cool, until 10.5 -mL y. each 15 bes ntil /ith add 5.2. rom tones, : 1238, essary [more rcially idated D2574 E < 3.2 Remove the cotton swab soaked with broth and [ |aje in a tube of sterile tryptone-glucose extract broth, transfer the inoculated broth to the sterile broth by pressing L swab against the inside wall of the tube. *5 3 3 Remove the cotton swab and incubate the broth iJture at 27 to 28"C for 24 h. c 5 3.4 Soak a second sterile cotton swab in the broth added tbe culture of Pseudomonas aeruginosa described in 5.3.1. f?eove the cotton swab soaked with broth and transfer the Lculated broth to the surface of a tryptone-glucose extract slant prepared in 5.1 by pressing the swab gently on top Tfthe asar surface. Incubate slant at 27 to 28C for 24 h or ^jtil luxuriant colony growth is observed on the agar surface. Label as culture of Pseudomonas aeruginosa ATTC No. 10145 and store in a refrigerator at 10 to 13C until 5.3.1 is -peated for a future test. 5.3.5 Soak a sterile cotton swab in the inoculated broth culture following the incubation period described in 5.3.3. 5.3.6 Remove the swab and prepare a second broth culture by repeating 5.3.2 and 5.3.3. 5.3.7 Following the incubation period, use the broth f culture prepared in 5.3.6 to proceed as described in Section' 6. 5. Procedure 6.1 Preparation ofSpoiled Paint: 6.1.1 Transfer the well-shaken broth culture prepared in 5.3.6 to the 1-qt (945-mL) sample of paint (see 4.3). Shake the inoculated paint well before proceeding. 6.1.2 Incubate the paint at 27 to 28C for 1 week. 6.1.3 To determine whether or not the paint contains bacteria at the end of the incubation period, use a sterile cotton swab to transfer a specimen of paint to the surface of a tryptone-glucose agar slant. Incubate agar slant at 27 to 28C for 72 h. If colonies ofPseudomonas aeruginosa appear on the agar surface, paint is satisfactory for use as spoiled paint in 6.4.1. If colonial growth ofPseudomonas aeruginosa does not appear on the surface, repeat 6.1.1 and 6.1.2. 6.2 Preliminary Examination ofPaint Under Test: 6.2.1 Examine the can for evidence of swelling. If the can is swollen, exercise caution in removing the lid. 6.2.2 Remove the lid and smell the contents of the can. Deterioration of paint by microorganisms is often character ized by distinct odors. Such odors may be either putrefactive or fermentative. 6.2.3 Observe the contents of the can for the presence of stringy structures characteristic of the presence of certain microorganisms. 6.2.4 Observe the contents for noticeable losses in vis cosity. This physical change frequently occurs as the result of microbiological deterioration. 6.3 Determination ofPresence or Absence ofLiving Micro organisms in Paint Under Test: 6.3; 1 Soak a sterile cotton swab in the paint under test. Remove excess paint by pressing gently against inside of container. 6.3.2 Transfer the test paint to the surface of a tryptoneglucose agar slant by pressing the swab gently on the agar surface. 6.3.3 In order to obtain duplicate agar slants, repeat 6.3.1 and 6.3.2. 6.3.4 Incubate the inoculated agar slants at 27 to 28C for a minimum of 1 week. 6.3.5 If colonial growth of bacteria is observed on the agar surface at the end of the incubation period, the test is complete and may be reported in accordance with Section 7. 6.3.6 If colonial growth of bacteria is not observed on the agar surface at the end ofthe incubation period, continue the test as described in 6.4. 6.4 Challenging Test Paint by Inoculation: 6.4.1 To 100 g of the paint under test, add 1 g of pant spoiled in 7.1. 6.4.2 Incubate the paint for 6 weeks at 27 to 28C. 6.4.3 At the end of24,48, 72 h and 1 week of incubation and once each succeeding week throughout the incubation period, soak a sterile cotton swab in the paint. Remove excess paint by pressing against the side of the container and transfer the paint to the surface of a tryptone-glucose agar slant. 6.4.4 Incubate the agar slant at 27 to 28C for 1 week and observe the presence or absence of colonial growth of bacteria. 6.4.5 At the end of 6 weeks add an additional 1 g of paint spoiled in 6.1. Incubate for 2 weeks at 27 to 28C and repeat 6.4.3 and 6.4.4. 7. Report 7.1 Report the following information: 7.1.1 Results of observations noted under 6.2. 7.1.2 Presence or absence of living microorganisms in the paint as received, and after it has been inoculated (or reinoculated) with a sample of spoiled paint. 7.1.3 If living microorganisms are found in the paint as received, or after inoculation (or reinoculation), the paint shall be reported as "not resistant in the container to attack by microorganisms." 7.1.4 If living organisms are not found, the paint shall be reported as "resistant in the container to attack by microor ganisms." 8. Precision and Bias 8.1 No statement is made about either the precision or bias of this test method for measuring the resistance of emulsion paints in the container to attack by microorgan isms, since the result merely states observations of the paint under test and presence or absence of living microorganisms in the paint as received or after inoculation. 325 DU P050297508 02574 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited either tor revision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. r ? 1. Scop. 1.1 T discolor; 1.2 T \ ations, 5< ! address | the resp appropr, applied: 2. Refei 2.1 A D 172 off D 192 G24 Un 3. Sum; 3.1 T 5 ings is masked At the . panels e 4. Sign: 4.1 C accepta1 In desi? substra will re; methoc light oi 5. App 5.1 L 6. Test 6.1 F approxi glass or N' f include: j 326 ' 1 This: and Relat mittee DO Current published zAnnu 3 Annu DUP050297509 Designation: D 2620 - 87 Standard Test Method for Light Stability of Clear Coatings1 This standard is issued under the fixed designation D 2620; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovai j, Scope 1.1 This test method covers the determination of the discoloration of clear coatings by sunlight through glass. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents * 2.1 ASTM Standards: D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials2 D1925 Test Method for Yellowness Index of Plastics3 G24 Practice for Conducting Natural Light Exposures Under Glass2 coating which would not be lifted by the clear topcoat. (A baking enamel with the composition of 30% melamine formaldehyde resin and 70 % of the phthalie anhydride/coconut alkyd resin with 3 Ib/gal (1.36 kg/L) of titanium dioxide, per. gallon has been found satisfactory.) (3) The substrate intended for use with the clear coating. The light stability of the substrate may be determined by including an extra test panel without a clear topcoat. 6.2 Prepare specimens of the test materials by applying the coatings on the test panels to a dry film thickness of 2 0.2 mil (50 5 pm). 6.3 Prepare a reference specimen, representing a material . of known, performance in this test, with each set of test specimens. 6.4 Record the panel preparation details: method of coating application, baking conditions, film thickness, etc. These details will be established by mutual agreement between purchaser and seller in accordance with the type of product and its intended use. 3. Summary of Method 3.1 The effect of sunlight on discoloration of clear coat ings is determined by exposing under glass, coated panels masked at one end, to natural sunlight for a specified time. At the end of the exposure, the mask is removed and the panels evaluated for degree of discoloration. 7. Conditioning 7.1 Unless otherwise specified, condition the coated panels at 73.5 3.5F (23 2C) and 50 5 % relative humidity for 48 h if baked, or 7 days if air dried. 4. Significance and Use 4.1 Color change, particularly yellowing, is not generally acceptable to users of coatings when it is readily noticeable. In designing clear coating systems for interior use on various substrates, it is of interest to know how well the clear coats will resist color change caused by ambient light. This test method permits the evaluation of the effect of natural indoor light on the color stability of clear coatings. 5. Apparatus 5.1 Exposure Cabinet as described in Practice G 24. 6. Test Specimens 6.1 For each clear coating under test, use one test panel approximately 3 by 5 in. (75 by 125 mm) of white carrara glass or other specified substrate material. N' 1--Other materials that may be considered for this purpose include: (/) White ceramic tile. (2) A white pigmented, light-stable 8. Procedure 8.1 Prior to exposure, mask one-half of each test panel with aluminum foil to exclude sunlight from the other half of the coating. N' 2--The tape used to attach the mask to the panel should not extend over the edge of the mask but should extend beyond the ends of the mask and stick to the rear of the panel, thereby holding the mask in position. This will prevent contact between the tape and the finish and eliminate the possibility of staining from the tape. 8.2 Mount the test specimens in the glass-covered expo sure cabinet continuously 24 h a day for the specified period of exposure. It is recommended this period should be approximately 5 weeks, since longer periods of exposure do not significantly change the results. N' 3--In cooperative tests, exposure of nitrocellulose lacquers, cellulose acetate butyrate lacquer, and low-bake alkyd enamel for 22 weeks did not show significantly greater discoloration than after exposure for 5 weeks. 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.55 on Factory-Applied Coatings on Preformed Products. Current edition approved May 29, 1987. Published July 1987. Originally Published as D 2620 - 67. Last previous edition D 2620 - 68 (1981)*'. 2 Annual Book ofASTM Standards, Vol 14.02. 3 Annual Book ofASTM Standards, Vol 08.02. 9. Interpretation of Results 9.1 Visual ratings of the degree of discoloration may be made. However, it is preferred that an instrumental method be used as described in Test Method D 1925, (see Test Method D 1729). 327 - < DUP050297510 If, 8 ! D2620 10. Color Changes Not Caused by Light' 10.1 In many cases atmospheric conditions (temperature, humidity, reactive gases) may produce significant color changes even without the presence of light. An indication as to whether or not side effects are operating may be obtained by retaining unexposed a duplicate set of specimens in the laboratory. A difference in color between the unexposed specimens and the covered portion ofthe exposed specimens indicates that the material has been affected by some agent other than light. 10.2 Further clarification regarding atmospheric effects may be obtained by simultaneously exposing a duplicate set of test specimens in another cabinet ofthe same type used in the light exposures but with the glass covered with an opaque material so that the light is excluded. 11. Report 11:1 Report the following information: 11.1.1 Visual ratings or instrumental values for degree of I discoloration of coatings or both, 11.1.2 Date and location of exposure, 11.1.3 Length of exposure, 11.1.4 Substrate used, 11.1.5 Details of panel preparation, and 11.1.6 Conditioning of panels prior to testing. 12. Precision 12.1 Because of the many variations in visual rating 0f | discoloration, meaningful estimates of precision cannot beA given. In cooperative tests, however, fairly good agreementf was obtained by the various cooperators in the visual rating i of the test panels. w TheAmerican Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ofinfringement of such rights, are entirely their own responsibility. 1. tic ini sp' This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five /ears and ifnotrevised, eitherreapproved or withdrawn. Yourcomments are invitedeither tor revision olthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair homing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. Hi !!& 328 DUP05029751 1 ijOjM Designation: D 2621 - 87 Standard Test Method for Infrared Identification of Vehicle Solids From Solvent Reducible Paints1 This standard is issued under the fixed designation D 2621; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the qualitative characteriza tion or identification of separated paint vehicle solids by infrared spectroscopy within the limitations of infrared spectroscopy. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish. appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1467 Guide for Testing Fatty Acids Used in Protective Coatings2 D1962 Test Method for Saponification Value of Drying Oils, Fatty Acids, and Polymerized Fatty Acids2 D2372 Method of Separation of Vehicle from Solvent- Reducible Paints3 E 131 Definitions of Terms and Symbols Relating to Molecular Spectroscopy4 E 275 Practice for Describing and Measuring Performance of Ultraviolet, Visible, and Near Infared Spectropho tometers4 3. Definitions 3.1 For definitions of terms of symbols, refer to Defini tions E 131. 4. Summary of Test Method 4.1 Infrared spectra are prepared from dried films of isolated paint vehicles. Vehicle types are identified by comparing the spectra to a collection of reference infrared spectra. 1 This lest method is under the jurisdiction of ASTM Committee D-l on Faint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Faints and Faint Materials. Current edition approved June 26, 1987. Published August 1987. Originally published as D2621 -67T. Last previous edition D 2621 -69 (1981)". 1 Annual Book ofASTM Standards, Vo! 06.03. 3 Annual Book cfASTM Standards, Vol 06.01. * Annual Book cfASTM Standards, Vol 14.01. 5. Significance and Use 5.1 The ability to qualitatively identify paint vehicles is useful for characterizing unknown or competitive coatings, for complaint investigations, and for in-process control. 6. Apparatus 6.1 Spectrophotometer--A recording double-beam in frared spectrophotometer with a wavelength range from at least 2.5 to 15 pm and a spectral resolution of at least 0.04 pm over that range. See Practice E 275. 6.2 Demountable Cell Mount with NaCl window. 6.3 Vacuum Drying Oven thermostatically controlled to operate at 60 2C. A water aspirator vacuum source is satisfactory. 6.4 Oven, Gravity or Forced Draft, capable of maintaining temperature from. 105 to 1 ICC. 7. Procedure 7.1 Place the vehicle, separated from the paint in accord ance with Method D 2372, on a NaCl window and spread to form a uniform film. The thickness of the film should be such that when the infrared spectrum is recorded the transmittance of the strongest band falls between 5 and 15 % (Note). Dry the film in an oven at 105 to 110*C for 15 min and cool in a desiccator. Inspect the film visually for defects such as bubbles, wrinkles, contamination, etc. If defects are present, cast another film. If easily oxidizable substances are present such as tung, oiticica, or linseed oils, the film should be dried at 60 25C in a vacuum oven for 1 h. If solvents of low volatility such as cyclohexanone or isophorone are present, the film may need to be dried for several hours in a 60C vacuum oven. N' --Numerous procedures and variations may be used to obtain a film on which to prepare a suitable spectrum. These include liquid mounting between two NaCl plates, transmission through free films, and reflectance from highly polished surfaces. 7.2 Immediately record the infrared spectrum from 2.5 to 15 pm so that a spectral resolution of 0.04 pm is maintained throughout that range (methods for achieving this resolution will vary according to the directions of the manufacturer of the instrument used). 7.3 Compare the spectrum obtained with reference spectra prepared from nonvolatile vehicles of known compo sition (see Annex Al) or consult other published spectra available in the literature (Annex A3). Interpret the spectrum on the basis of available information, recognizing certain limitations- of infrared spectroscopy, and qualifying the interpretation accordingly (Annex A2). 329 DUP050297512 D 2621 Wavelength, jtm 2.9 3.4 to 3.5 5.8 6.2, 6.3. 6.6, 6.7 6.9. 7.3 7.5 to 9.4 8.6 9.6. 13.5,14.3 TABLE 1 Correlation of Absorption Banda in Alkyd Spectra Wavenumbers, cm-1 Group Vibration ~~ 3448 2941 to 2857 1724 1613, 1587,1515, 1493 1449. 1369 1333 to 1063 1163 1042,741,699 0--H stretch ; alkane C--H stretch ester, 0=0 stretch r.. skeletal In-plane aromatic C=C aliphatic C--H bending ester, C--0--C stretch (o-phthalate ester) ester, C--0--C stretch (fatty acid ester) out-of-plane aromatic C--H bending denoting o-disubstituted benzene ring. ! ANNEXES (Mandatory Information) Al. INFRARED SPECTRA OF NONVOLATILE VEHICLES OF KNOWN COMPOSITION A 1.1 A set of reference infrared spectra on grating and prism is reproduced on the following pages. A2. CONSIDERATIONS IN THE INTERPRETATION OR INFRARED SPECTRA OF NONVOLATILE VEHICLES SEPARATED FROM SOLVENT-TYPE PAINTS INTRODUCTION stretc tions ester A2 Thest of ri: adjac A2 A2 the a sfflou unmc shoul Thee withii "shor A2. matic presei A2. usual ficatk requii acids dures The infrared spectra of vehicles recovered from whole paint are presented in Annex Al. The aim of this compilation is to aid those using Test Method D 2621 in the practical interpretation of.the spectra they obtain. The spectra are compiled with one representative spectrum of each vehicle presented in both a prism and a grating format. In the discussion of the spectra, the general assignment refers to the first spectrum. The subsequent spectra discussion will include only- those bands which aid in the identification of the particular modifications being illustrated. In addition, some practical information is provided where it is believed to be helpful to the analyst. In general^ previously noted band assignments are not repeated. The data compiled here were obtained from spectra , prepared on very carefully calibrated instruments. In comparing them to spectra prepared in any given laboratory, it is expected that the wavelength values of absorptiqn bands may differ slightly depending upon the calibration of the instrument used. GROUP I-ALKYDS A2.1 Spectrum 1: Ortho-Phthalic Alkyd, Medium Oil Length A2.1.1 2.9-\im Region (3448 cm"1)--the 2.9-pm band in alkyds is due to the O--H stretching vibration. This is usually attributed to the unesterified hydroxyl OH on the polyhydric alcohol used in manufacturing the alkyd. This absorption is known to increase on drying of unsaturated oil modified alkyds due to oxidation of the double bonds. This absorption band can be used to determine the hydroxyl number of alkyds. A2.1.2 3.3 to 3.6-\im Region (3030 to 2778cm~1)--The bands in this area are all due to aromatic and aliphatic G--H stretching vibrations. / A2.1.3 5 to 6-\un Region (2000' to 1667 The1 5.8-pm band in alkyds is due to the combined 0=0 stretch of the phthalate and fatty acid esters. Unreacted phthalic . anhydride, if present, may be detected by the appearanceofa sharp absorption band at approximately 5.6 pm (1786 cm"1). Free carboxyl groups (due to unreacted fatty acid or incompletely reacted phthalic acid) may often be detected by the appearance of a shoulder on the high wavelength (low frequency) side of the ester carbonyl band... A2.1.4 6.2 to 6.4-\im Region (1613 to 1563 cm~Ij--The doublet appearing in this region of the spectrum is due to vibrations associated with the double bonds in an aromatic ring. The band shape and position of this doublet is characteristic of non-oil modified, ophthalic alkyds. A2.1.5 6.8 to 6.9-\un Region (1470 to 1449 cm"1)--This absorption is produced by C--H bending vibrations , of methylene (scissoring deformation) and methyl (asymmet- rical deformation) groups, in the alkyd. The: intensity of this.' absorption band will vary with oil length. `' A2.1.6 7.2 to 7,3-jim Region (1389 to 1370 cm~!)--TW absorption band is due to the C--CH3 symmetrical deforma tion vibration, and is produced by-the methyl groups on the fatty acid chains. A2.1.7 7.5 to 10.0-\im Region (1333 to 1000 cm"1)--The absorption bands in this region are due to the C--O--C f [ j i | \ A2.2 A2. A2. (1163 oil ler A2_3 A2. Conji A2. the 1( Specti (in su conjt and A2.4 A2 A2 A2. A2. ring A2. of am an iso ence c to a s' noting cm'1) dm (7 A2.5 A2. vibrati 330 DUP05029751 3 ring. ICLES ted by 1 (low --The due to bmatic blet is --This ons of mmetof this. --This formaon the )--The -O--C # D 2621 ^etching vibrations of the phthalate ester. These absorp tions are most strongly influenced by the acid portion of the ggter rather than the alcoholic portion. A2.1.8 13.5 and 14.2-p.m Regions (741 and 704 cm~`)-- fbese two bands are due to out-of-plane bending vibrations 0f ring hydrogens of aromatic compounds having four adjacent hydrogens (orthodisubstitution). A2.1.9 Comments: A2.1.9.1 Note that in oil-modified alkyds, the intensity of the absorption at 8.6 pm (1163 cm-1) is indicative of the amount of oil modification or oil length of the alkyd. In unmodified alkyds, this band may be little more than a side shoulder on the 8.9-pm (1124-cm-1) C--O--C absorption. The correlation to oil length is only a very general one in that within a given group of alkyds one may say a sample is a "short," "medium," or "long" oil type. A2.1.9.2 Alkyd spectra generally reveal little or no infor mation concerning the type of combined oil or polyol present. A2.1.9.3 Identification of polyol and unsaponifiables may usually be accomplished by infrared examination of saponir fication fractions. Identification of the oil acids used usually requires gas chromatographic analysis of the methylated fatty acids recovered by saponification. (For saponification proce dures see Test Methods D 1467 and D 1962.) A2.2 Spectrum 2: Ortho-Phthalic Alkyd, Long Oil Length A2.2.1 8.6 pm (1163 cm-1); fatty acid ester C--O--C A2.2.2 Comments--Note the difference in the 8.6-pm (1163-cm-1) peak compared to Spectrum 1, due to increased oil length. A23 Spectrum 3: Ortho-Phthalic Alkyd, Tung Oil Modified A2.3.1 10.12 jun (988 cm-1); --C=C--C=C--G=C-- Conjugated triene unsaturatiom A2.3.2 Comments--Note the difference in band shapes in the 10 to 10.4-|um region (1000 to 962 cm-1) compared to Spectra 1 and 2. Absorption due to conjugated unsaturation (in such oil types as tung, oiticica, dehydrated castor, and conjugated safflower) occurs here. Oil types used for alkyds l and 2 contain only isolated double honds. A2.4 Spectrum 4: Ortho-Isophthalic Alkyd A2.4.1 7.8 pm (1282 cm1) isophthalate ester C--O--C A2.4.2 8.2 pm (1220 cm-1) isophthalate ester C--O--C A2.4.3 8.9 pm (1124 cm-1) isophthalate ester G--O--C A2.4.4 13.7 pm (730 cm-1) meta-disubstituted benzene ring A2.4.S Comments--The spectrum of this alkyd is typical ofan isophthalic alkyd. The major band that identifies this as an isophthalate is the 13.7-pm (730:cm-1) band. The pres ence of orthophthalic alkyd can be suspected by comparison to a straight isophthalic alkyd spectrum (see following) and noting the influence of the ortho-phthalate at 7.9 pm (1266 cm-1), 9.0 pm (1111 cm-1), 9.4 pm (1064 cm-1), and at 14.2 Hm (704 cm-1). ;. A2.5 Spectrum 5: Ortho-Phthalic Alkyd, Benzoic Add Modified A2.5.1 14.0 to 14.1 pm (714 to 709 cm-1); aromatic ring vibration where ring contains five adjacent hydrogens. Posi tion is characteristic of benzoate esters. A2.5.2 Comments--The band at approximately 14.0 pm (714 cm-1) is the identifying peak for this modification. Because of the o-disubstitution peak at 14.3 pm (699 cm-1) present in o-phthalates, it is difficult to observe this band when the benzoic acid modification drops below 3 %. A2.6 Spectrum 6: Ortho-Phthalic Alkyd, Para-Tertiary Butyl Benzoic Add Modified A2.6.1 8.4 pm (1190 cm-1) C--O--C p-tert. butyl benzoate A2.6.2 9.6 pm (1042 cm-1) C--O--C p-tert. butyl benzoate - A2.6.3 9.8 pm (1020 cm-1) C--O--C p-tert. butyl benzoate A2.6.4 11.7 pm (855 cm-1) aromatic ring substitution patterns A2.6.5 12.9 pm (775 cm-1) aromatic ring substitution patterns A2.6.6 Comments--The characteristic bands for the iden tification of the paratertiary butyl benzoic acid modification are the ll.7-pm (855-cm-1) and the 12.9-pm (775-cm-1) bands. The other absorption bands, although sharp and distinctive, can tend to be lost in the background of the spectrum when the modification drops below 2 to 3 %. A2.7 Spectrum 7: Ortho-Phthalic Alkyd, Tall Oil, Rosin Modified A2.7.1 12.3 pm (813 cm-1) abietic acid ring vibration A2.7.2 Comments--The curve shows only a very slight depression at 12.3 pm (183 cm-1). In general, the band is never very intense and1, if suspected, the presence of rosin is readily confirmed by a Lieberman-Storch spot test. Note also the obscured nature of the 6.3 to 6.5-pm (1587 to 1538cm-1) region. This is most likely due to the salt or "soap" formation with the adds present in the system and the pigment used. A2.8 Spectrum 8: Ortho-Phthalic Alkyd, p-Phenyl Phenol Modified, 1' A2.8.1 11.4 pm (877 cm-1) associated with substituted aromatic rings A2.8.2 12.1 pm (826 cm-1) associated with substituted aromatic rings A2.8.3 13.1 pm (763 cm-1) associated with substituted aromatic rings A2.8.4 14.4 pm (694 cm-1) associated with substituted aromatic rings A2.8.5 Comments--The main identifying band is the 13.1-pm (763-cm-1) band, The other bands are less distinc tive, especially the 14.4-pm (694-cm-1) area. It is always best to consider, the positions of the 3 or 4 absorptions in the far end of the curve as a group in assigning the modifying structure. . A2.9 Spectrum 9: Ortho-Phthalic Alkyd, Styrene Modified A2.9.1 6.7 pm (1493 cm-1) aromatic ring vibration A2.9.2 13.2 pm (758 cm-1) monosubstituted aromatic (5 adjacent ring hydrogens) A2.9.3 14.3 pm (699 cm-1) monosubstituted aromatic (5 adjacent ring hydrogens) 331 DUP050297514 D 2621 A2.9.4 Comments--The very general forebroadening in A2.14.2 12.3 pm (813 cm"1) triazine ring vibration the 13 to 13.3-pm (769 to 758-cm"1) area of the ortho A2.14.3 Comments--A melamine modification is always: substitution band is characteristic of styrene modification. distinguishable from the urea-formaldehyde modification ig The 14.3-pm (699-cm"1) absorption that obscures the nor that it lacks the 6.1-pm (1639-cm"1) absorption and contains mally present small 14.3-pm (699-cm"1) band is the primary the 12.3-pm (813-cm-1) triazine ring vibration. styrene absorption. Note also the sharp 6.7-pm (1493-cm"1) peak which is associated with the presence of an aromatic. A2.10 Spectrum 10: Ortho-Phthalic Alkyd, Vinyl Toluene A2.15 Spectrum 15: Ortho-Phthalic Alkyd, Benzoguana. mine-Formaldehyde Modification Modified A2.10.1 6.6 pm (1515 cm"1) aromatic ring vibrations A2.10.2 6.7 pm (1492 cm"1) aromatic ring vibrations A2.10.3 11.4 pm (877 cm'1) meta-disubstituted aromatic A2.10.4 12.3 pm (813 cm"1) para-disubstituted aromatic A2.10.5 12.8 pm (781 cm"1) meta-disubstituted aromatic A2.10.6 14.2 pm (704 cm"1) meta-disubstituted aromatic A2.10.7 Comments--The general pattern of peaks at the end of the spectrum is characteristic for vinyl-toluene modification. They arise from the meta-para mixed isomers.. A2.15.1 6.3 pm (1587 cm"1) aromatic ring vibration A2.15.2 6.5 pm (1538 cm"1) C=N A2.15.3 12.1 pm (826 cm"1) characteristic band for ) benzoguanamine derived modification A2.15.4 12.8 pm (781 cm-1) characteristic band f0r benzoguanamine derived modification A2.15.5 14.2 pm (704 cm"1) characteristic band for benzoguanamine derived modification A2:15.6 Comments--The G=N band occurs at a slightly ; lower wavelength than in the melamine resins. The band at-: A2 A2.ll Spectrum 11: Ortho-Phthalic Alkyd, Acrylonitrile Modified ~ A2.11.1 4.5 pm (2222 cm"1) feN nitrile stretching 12. l pm (826 cm"1) rather than at 12.3 pm (813 cm"1) also 1 helps to distinguish between the two types of triazine based resins. -i A2 vibration A2.11.2 Comment--The 4.5-pm (2222-cm"1) band is the A2.16 Spectrum 16: Ortho-Phthalic Alkyd, Hex*. outstanding feature characteristic of an acrylonitrile modifi Methoxymethylmelamine Modified cation. A2.16.1 9.3 pm (1075 cm"1) C--O--C ether :K 2.12 Spectrum 12: Ortho-Phthalic Alkyd, Bis-Phenol Epoxy Modified A2.12.1 8.4 pm (1190 cm"1) aromatic C--O--C A2.12.2 10.9 pm (917 cm"1) terminal epoxy grouping A2.I6.2 Comments--The presence of hexamethoxymethylmelamine can be observed in the spectrum of aul ortho-phthalic-alkyd by its influence at 6.5 pm (1538 cm~!jf 6.7 pm (1493 cm"1); 9.3 pm (1075 cm"1); 9.9 pm (lOffil cm"1); 10.9 pm (917 cm"1); 11.5 pm (870 cm"1); and 12,3`* --CH--CH2 \/ o A2.12.3 12.1 pm (826 cm"1) para-disubstituted aromatic. A2.12.4 Comments--The band at 10.9 pm (917 cm"1) is due to the weakly absorbing terminal epoxy group. The I2.1-pm (826-cm"1) absorption is due to die bis-phenol backbone of the epoxy polymer. The band at 8.4 pm (1190 cm"1) is also always present in conjunction with the 12:1-pm (826-cm-1) band. pm (813 cm"1). .. ' - -^ . 'I A2.17 Spectrum 17: Ortho-Phthalic Alkyd, Rosin-Maleic -, Adduct Modified A2.17.1 5.4 pm (1852 cm"1) --C=0 stretching vibrios tions associated with anhydrides V A2.17.2 5.6 pm (1786'cm"1) --C=0 stretching vibra-',, tions associated with anhydrides - A2.17.3 Comments--The most characteristic absorptions! are the ones listed above which cause multiple bands in tl " A2.13 Spectrum 13: Ortho-Phthalic Alkyd, Urea-Formal carbonyl area. The presence of the rosin-maleic adduct can ip dehyde Modified also be seen at 10.6 pm (943 cm"1); 10.9 pm (917 cm-1); . A2.13.1 3.1 pm (3226 cm"1) N--H stretching vibration. A2.13.2 6.1 pm (1639 cm"1) amide linkage band A2.13.3 6.6 pm (1515 cm"1) amide linkage band 11.7 pm (855 cm"1); and 12.2 pm (820 cm"1). These bands 1 are generally found in all rosin-maleic adducts even if slightly:;; changed in intensities. 4lt A2.13.4 9.3 pm (1075 cm"1) --C--O--C ether A2.13.5 13.0 pm (769 cm"1) unknown (but present in all urea-formaldehyde resins). A2.13.6 Comments--The presence of urea-formaldehyde A2.18 Spectrum 18: Ortho-Phthalic Alkyd, Vinyl Chloride;,Acetate Modified . . f-s;ssfjp Ifil i in an o-phthalic alkyd can always be observed in the spectrum by its influence at the wavelengths listed above. A2.18.I 7.0 pm (1428 cm"1)--CH2-- A2.18.2 8.0 pm (1250 cm"1) --CH in --CHQ-- The general curve shape is somewhat depressed throughout. A2.18.3 14.5 pm (690 cm"1) C--Cl The 3.1-pm (3226-cm"1) absorption appears as'a shoulder A2.18.4 Comments--The most characteristic features off on the O--H stretch at 3.0 pm (3333 cm"1). this spectrum are the 8 to 8.1-pm (1250 to 1234~cm"!|| absorption and the-very broad band peaking at approxi A2.14 Spectrum 14: Ortho-Phthalic Alkyd, ,,Meiamin&. mately 14.5 pm (690 cm"1). A general depression of Formaldehyde Modified entire curve is noted between 7.0 pm (1428 cm"1) and 1G. A2.i4.1 6.5 pm (1538 cm"1) G=N pm (1000 cmfr1). 332 DUP050297515 tion i is always fication in d contains nzoguana- ration band for band for band for t a slightly le band at :m-1) also zine based !, Hexa- imethoxyum of an >38 cm-1); jim (1010 ; and 12.3 D2621 ^2.19 Spectrum 19: Ortho-Phthalic Alkyd, Phenyl Siloxane Modified A2.19.1 7.0 Jim (1429 cm-1) aromatic silicon bond A2.19.2 8.8 Jim (1136 cm-1) Si--O--Si A2.19.3 10.0 jim (1000 cm-1) aromatic silicon bond A2.I9.4 14.4 jxm (694 cm-1) mono-substituted aromatic A2.19.5 Comments--The general influence of the pres ence of silicone is seen in the depressed area from 8.8 pm 136 cm-1) to 10.0 jim (1000 cm-1). A2.20 Spectrum 20: Ortho-Phthalic Alkyd, Siloxane Modified A2.20.1 7.9 jim (1266 cm-1) --Si--CH3 A2.20.2 12.5 jim (800 cm-1) --(CH3)2--Si Methyl A2.21 Spectrum 21: Ortho-Phthalic Alkyd, Nitrocellulose Modified < A2.21.1 6.1 jim (1639 cm-1) R--O--N02 stretching vi bration A2.21.2 7.8 jim (1282 cm-1) R--O--N02 stretching vi bration A2.21.3 9.5 jim (1053 cm-1) general C--O--C ether from the cellulose ring A2.21.4 11.9 jim (840 cm-1) low-frequency vibrations associated with R--O--N02 A2.21.5 Comments--The most prominent absorptions are the 6.t-jim (1639-cm-1) band and the very broad 11.9-jim (840-cm-1) peak. An additional reliable feature of nitrocellulose is the ether linkage which causes a general depression in the mid-section of the spectrum. A2.22 Spectrum 22: Ortho-Phthalic Alkyd, Urethane Mod ified A2.22.1 5.8 pm (1724 cm-1) R--NH--CO--OR amide I band A2.22.2 6.3 Jim (1587 cm-1) aromatic vibration (in aro matic di-isocyanate systems) A2.22.3 6.5 jim (1538 cm-1) amide II band, C--N A2.22.4 12.3 jim (813 cm-1) 1,2,4 tri-substitution (in systems with toluene di-isocyanate) A2.23 Spectrum 23: Isophthalic Alkyd, Medium Oil Length A2.23.1 6.2 |im (1613 cm-1) ring unsaturation A2.23.2 13.8 jim (725 cm'1) meta-disubstitution band A2.23.3 Comments--Note the change from a doublet in the 6.2-jim (1613-cm-1) region to the singlet. The 13.8-|im (725-cm-1) band is characteristic for isophthalic alkyds. A2.24 Spectrum 24: Tere-Phthalic Alkyd, Medium Oil Length A2.24.1 8.6 jim (1163 cm-1) C--O--C A2.24.2 9.8 jim (1020 cm-1) C--O-C A2.24.3 Comments--The tere-phthalate spectrum is iden tified mainly by the 8.6-jim (1163 cm-1) and 9.8-pm (1020 cm-1) peaks combination in conjunction with a 13.8-jim (725 cm-1) peak position. A2.2S Spectrum 25: Ortho-Phthalic Alkyd, Chlorendic Acid Modified A2.25.1 Comments--The overall appearance of the ab sorption band pattern in this spectrum is characteristic of this modification. >in-Maleic ing vibra- :ng vibra- sorptions ids in the Iduct can 7 cm-1); ese bands < if slightly 1 Chloride- features of 234-cm-1) ,t approxiion of the ) and 10.0 333 DUP050297516 DUP050297517 D 2621 iXJMWLUHSNWiL 335 DUP050297518 4SD) D 2621 336 A DUP05029751 9 D 2621 i ? i i $ i WAVELENGTH (MICRONS) i i i I 3 I I 337 DUP050297520 DUP05 02 97521 # D 2621 DU P050297522 DUP050297523 D2621 ^ A/ M 1^*- 1 ^ |,- Fii"- ' - -{(- r -^i-- WAtUK)1M " >04 i|Tir*r j; r..?. ..n..: "ST^TI -- :iE :zPV rf&. 4- : J;:; l ) pit1" ^ '*j,j ' wl p'i'Mt ; ,I|,j-| ,:i I'r-- s?i t jil- pi |E nf -- * | p `|j- - -J-- -- -- 41 -- r -f 11 ' H irr ki ::... .;.:j.v: : :;j. : -:-p U, .... . 1.... : r It 44 "4 K-t T-- ' ;F ...j" -- - :;:f- .... 1WAVtNUMKK CM . ijt j TTT'l~ FTTP W-1.; M 4- -f; 4 Y -Ay. 4ii aA -A- #4 Mij- --p-T*1* it r-p .J ft. .!-- ! 1 'rM H1 " V Si;-- m rt- G; : - 1 IjPjg 4- r i ,ju irHsisi ...j;:!. SPECTRUM It*. K 4 CRA INC 341 xtti DUP050297524 D U P050297525 # D 2621 2.5 3 45 WAVELENGTH (MICRONS! 6 78 9 10 12 15 20 30 4050 -4000 3500 3000 2500 2000 1800 1600 1400 1200 1000 8CO 600 400 200 FREQUENCY (CM'l TRANSMITTANCE (PERCENT) 343 DU P050297526 \ 5i t i f DU P05 02 97527 4|K" 2621 2.5 3 45 WAVELENGTH (MICRONS) 6 7 8 9 10 12 15 20 30 40 50 TRANSMITTANCE (PERCENT) 345 DU P0502 97528 #02621 346 DUP050297529 WAVELENGTH (MICRONS) DUP050297530 DU P050297531 # D 2621 DUP050297532 WAVELENGTH (MICRONS) FREQUENCY (C M `) DUP050297533 # D 2621 DUP050297534 WAVELENGTH (MICR0N5) WAVELENGTH (MICRONS) DU PO50297535 WAVELENGTH (MICRONS) DUP050297536 DUP0502 97537 # 0 2621 r WAVEIENOTH (MICRONS) | 357 DUP05 029 7538 FREQUENCY (CM') WAVELENGTH (MICRONS) DUP0502 97539 # D 2621 A3. SOURCES OF INFRARED SPECTRA OF KNOWN MATERIALS (1) Weinberger, L. A., and Kagarise, R. ., Infrared Spectra ofPlastics and Resins, U. S. Department of Commerce. OTS Bulletin No. PB 111438. (2) Brown, W. H., et al, "Infrared Spectroscopy--Its Use as an Analytical Tool in the Field of Paints and Coatings," Official Digest, March 1963. (3) Perfetti, B. N., and Miller, J. H., "Optical Instru mental Analysis of Organic Coatings," Official Di gest, August 1961. (4) Nyquist, R. A., Infrared Spectra of Plastics and Resins, 2nd Ed., The Dow Chemical Company, Midland, Mich., 1961. (5) Haslam, J., and Willis, H. A., Identification and Analysis ofPlastics, D. Van Nostrand Co., Inc., New York, N. Y,, 1965. (6) Secrest, P. J., "Infrared Studies of Phenolic Resins," Official Digest, February 1965. ~ (7) Sadder Commercial Infrared Spectra,- Sadtfer Re search Laboratories, Inc., Philadelphia, Pa. (8) Welcher, F. J., Ed., Standard Methods of Chemical Analysis, 6th Ed., D. Van Nostrand Co., Inc., Vol II B, 1963, p. 1709 - 21 (39 Spectra). (9) Clark, G. L., Ed., The Encyclopedia ofSpectroscopy, Reinhold Publishing Corp., 1960, p. 506 - 15 (104 spectra of pigments, binders solvents, and additives). (10) Hummel, D. O., Kunststoff-, Lack-Und GummiAnalyse, Carl Hanser Verlag, Munchen, 1958. (11) Hummel, D. O., Infrared Spectra ofPolymers in the Medium and Long Wavelength Regions, Vol 14, Polymer Reviews, Interscience Series, 1966. (12) Stimler, S. S,, and Kagarise, R. E., Infrared Spectra of Plastics and Resins: Part 2--Materials Developed Since 1954, NRL Report No. 6392, 1966. (13) Federation of Societies of Paint Technology, Infrared Spectroscopy, Its Use in the Coatings Industry. (14) Cain, Dorothy S., et al, Infrared Spectra of Plastics and Resins: Part 3--Related Polymeric Materials (Elastometers), Naval Research Laboratory Report No. AD 649 094, 1967. The American Society tor Testing and Materials fakes no position respecting the validity ofany patent lights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ot infringement of such rights, are entirely their own responsibility. This standard is subject to revision al any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprovedor withdrawn. Your comments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments wit! receive careful consideration at a meeting ot the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 flaca St.. Philadelphia, PA 19103. 359 DUP050297540 Designation: D 2691 - 88 Standard Test Methods for Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products1,2 This standard is issued under the fixed designation D 2691; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (r) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover the measurement of film thickness of dried coatings applied to a plane rigid substrate of wood or a wood-base material. These test methods apply to both opaque and clear coatings. They axe not recom mended for metal or glass substrates. Test Method A uses a .Vv WVv WWVn Vv Punch razor blade and Test Method B a microtome for cross sectioning. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to V/////////////////////////y\ Push Rod (felWioped) address all ofthe safety problems associated with its use. It is FIG. 1 One Type of Tool for Extracting Coated Wood Specimeni the responsibility of the user of this standard to establish appropriate safety and health practices and determine the 4:1. applicability of regulatory limitations prior to use. 2. Significance and Use removal intact within the punch. 3.3 Source ofOblique Illumination. 3.4 Hand Microtome (Method B). t'ft 2.1 This test method provides a precise, quantitative measurement of the thickness of a dried coating. It may be 4. Test Specimens used for quality control or monitoring of the production of 4.1 Specimens for microscopical measurement shall be coated wood products. extracted from the punch tool % means of a push rod 3. Apparatus inserted through the hollow shaft of its tube. The end of the push rod should be tipped with felt or other soft material so 3.1 Calibrated Monocular Compound Microscope, that the coated surface of the disk will not be damaged equipped with an optical system sufficient to provide sharp during extraction. resolution of the cross section to be examined. One system, consisting of a 16-mm objective and a 10-power filar micrometer eyepiece, resulting in a magnification of approx imately 100 diameters, has been found satisfactory. Other combinations of objectives and eyepieces and other magnifi cations may also be suitable, although magnifications above 200 diameters may result in distortion of the viewed cross section. 3.2 Toolfor Extracting Test Specimens--The tool may be similar in design to an ordinary cork borer, except that it shall be made of thicker walled tubing, hard enough to hold a keen cutting edge, and be fitted with a head suitable for pounding with a hammer (Fig. 1). A leather punch has been found satisfactory for this use. The tool shall make a circular cut approximately lh in. (12.7 mm) in diameter and Vt in. (3.2 mm) deep through the coating and into the substrate. A sidewise movement of the punch while firmly embedded in the substrate will dislodge the specimen and allow its 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility Of Subcommittee D01.S2 on Factory-Coated Wood Products. Current edition approved March 29, 1988. Published May 1988. Originally published as D 2691 - 68. Last previous edition D 2691 - 70 (I981)el. 1 This test method is presently under study for revision or replacement with an improved microscopical film thickness method. 5. Procedure 5.1 Prepare disks for microscopical examination and meas urement by either Method A or Method B. Either method of preparation will expose a cross section of coating and sub strate, including the extremes in film thickness resulting from variations in the wood surface or method ofapplication. 5.2 Method A, Cross Sectioning with Razor Blade--With a sharp razor blade carefully slice away parallel to the coated surface the substrate adhering to the coating until the disk is approximately Vie in. (1.6 mm) thick. Place the disk coated face down on a smooth, hard surface and cut in half by means of a slicing stroke with a fresh razor blade (Fig. 2). Cut in a direction perpendicular to the grain of the wood substrate and at right angles to the coated surface. 5.3 Method B, Cross Sectioning with Microtome: 5.3.1 With a sharp razor blade carefully slice away parallel to the coated surface the substrate adhering to the coating until tiie disk is approximately Vie in. (1.6 mm) thick. 5.3.2 Embed the thinned disk in molten paraffin3 which is 3 Paraplast, available from Fischer Scientific, 191 South Gulph Road, P.O. Box I, King of Prussia, PA 19406 melting point about 50 to 60'C, Ms been found satisfactory for this purpose. For clear films the addition of 0.5 g of Indigo to 200 mL of paraffin improves optical definition. 360 FIG. FIG. allowed surroun successi deposit 5.3.3 sides an 5.3.4 microto vertical to the c or to t should 1 chuck s embedc 5.3.5 of the k cut. Co protrud the mic approx; 5.3.6 disk wit obtaine plished. 6. Mic; 6.1 r aminati eling cl; a petri speclmt microsc recomn 6.2 I strate a DUP0502 97541 simens tall be sh rod of the trial so maged . meashodof 1 subulting ation. -With oated disk is coated talf by 2). Cut wood parallel toating hich is P.O. Box ea found go to 200 # D 2691 Disk fallowing removal from punch Trimmed disk \ Sectioned disk (ProcedureA) (Coated face down) FIG. 2 Coated Wood Specimens Before and After Trimming and Coating j Direction of View FIG. 3 Specimen Mounted in Clean Sand for Microscopical Examination (Method A) allowed to harden in a small mold to form a block which surrounds the disk on all sides. (The disk may also be dipped successively in the molten paraffin until a reasonably heavy deposit of wax is obtained.) 5.3.3 Trim the paraffin block with razor blade until the sides are parallel to the woodcoating surface. 5.3.4 Mount the trimmed block in a sliding-knife hand microtome4 in such a manner that the embedded disk is vertical with its cross-sectional edge facing and perpendicular to the oncoming knife edge. Cut perpendicular to the grain or to the machine direction of the specimen. The block should be firmly clamped between the jaws ofthe microtome chuck so that approximately one third of the diameter of the embedded disk protrudes. 5.3.5 Make successive cuts with a single sliding movement of the knife, raising the block by small increments after each cut. Continue sectioning until the clamped paraffin block protrudes no more than lAe in. (1.6 mm) above the jaws of the microtome chuck and the embedded disk is sectioned to approximately one half its diameter. 5.3.6 Examine the exposed cross section of the embedded disk with a hand lens to ascertain that a smooth cut has been obtained. If not, resume sectioning until this is accom plished. Do not measure within V32 in. (0.8 mm) of the edges of the disk, nof in areas where obvious deformation of the coating or substrate has occurred. 7. Report 7.1 Report the average film thickness computed from the ten random measurements as well as the maximum and minimum thicknesses measured to the nearest 0.1 mil (2.5 pm). 7.2 If a more extensive sampling procedure is employed, the report shall show the number of disks examined and the number of measurements per disk, in addition to the maximum, minimum, and average film thickness computed from all measurements. 8. Precision 8.1 Opaque Coatings: 8.1.1 Test Method A--On the basis of an interlaboratory test of this method in which operators in six laboratories tested 12 materials covering a wide range in film thickness, the within-laboratory standard deviation was found to be 0.26 mils with 72 degrees of freedom, and the betweenlaboratory standard deviation was found to be 1.03 mils with 60 degrees of freedom. Based on these standard deviations, the following criteria should be used for judging the accept ability of results at the 95% confidence level: 8.1.2 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 0.7 mils. 8.1.3 Reproducibility--Two results, each the mean of duplicate measurements, obtained by operators in different laboratories should be considered suspect if they differ by more than 3 mils. 8.1.4 Test Method B--On the basis of an interlaborary test of this method in which operators in three laboratories tested 12 materials covering a wide range in film thickness, the within-laboratory standard deviation was found to be 0.28 mils with 36 degrees of freedom and the betweenlaboratory standard deviation was found to be 0.66 mils with 24 degrees of freedom. Based on these standards deviations, the following criteria should be used for judging the accept ability of results at the 95% confidence level. 8.1.5 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 0.8 mils. 6. Microscopical Measurement 6.1 Mount the cross-sectional disk for microscopical ex amination by carefully mounting in parallel clamps, mod eling clay, or in clean sand held in a small container such as a petri dish (Fig. 3). Examine the edge-on view of the specimen by oblique overstage illumination. A focusable microscope lamp and a rotatable microscope stage are recommended for obtaining optimum viewing conditions. 6.2 Determine thickness of the coating above the sub strate at ten randomly selected points on the cross section. * A Spencer microtome (Catalog No. 900), available from American Optical, Warner-Lambert Co., Reichert Scientific Instrument Division, 201-T Tabor Rd, Morris Plains, NJ 07950 has been found suitable for this puipose. TABLE 1 Laboratory Standard Deviations of Opaque Coatings Standard Deviation Substrate Between Method A Method B Within Method A Method B Wood Hardboard or overlaid plywood 0.97 0.66 1.09 0.25 0.30 0.34 0.22 0.21 TABLE 2 Substrate Wood Hardboard or overlaid plywood Repeatability Method A 0.8 0.6 Method B 1.0 0.6 361 DUPO 50297 542 -Q269f 8.1.6 Reproducibility--Two results, each the mean of duplicate measurements, obtained by operators in different laboratories should be considered suspect if they differ by more than 2 mils. 8.2 Clear Coatings: 8.2.1 Test Method B--On the basis of an interlaboratory test of this method in which operators in six laboratories tested 16 materials covering a wide range in film thickness, the within-laboratory standard deviation was found to be 0.07 mils with 96 degrees of freedom, and the between- laboratory standard deviation was found to be 0.10 mils witjj 80 degrees of freedom. Based on these standard deviations n the following criteria should be used for judging the accept! ability of results at the 95% confidence level: i 8.2.2 Repeatability--Two results obtained by the same ; operator should be considered suspect if they differ by mom I than 0.2 mils. 8.2.3 Reproducibility--Two results, each the mean of duplicate measurements, obtained by operators in different j laboratories should be considered suspect if they differ by ; more than 0.3 mil. [ V The American Society for Tasting and Materials takes no position respecting the validity ofany patent rights assertedin connection with any item mentioned in this standard. Users of thliistandard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of. such-rights, areentirely thefr own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meet/ng ol the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your vieivs known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. , 1. Set ! u. 1 detern \ variet; precis extern iocluc r | prime disper ; cludet i an in< exteri i 1.2 probh user | healtl | limitc \ 2. Re 2.1 D1 c "; D; I ": -Lit: - . 362 | 3. S 3. detei i teste, is de liquii \ quoti \ Arch [ liquii such | sped ; mere ; the c i iT and R niittee Cm i publis 2A DU P050297543 3 mils wit(j deviations the accept' the saute er by more mean 0f n different i differ by Designation: D 2697 - 86 (Reapproved 1991)61 Standard Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings1 This standard is issued under the fixed designation D 2697; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon () indicates an editorial change since the last revision or reapproval. el N' --Keywords were added editorially in January 1991. 1, Scope 1.1 This test method is believed to be applicable to the determination of the volume of nonvolatile matter of a variety of coatings. An interlaboratory study to establish the precision of this test method included a water-reducible ^terior latex paint and three automotive coatings that included a solvent-reducible primer surfacer, water reducible primer surfacer, water reducible enamel topcoat, and acrylic dispersion lacquer topcoat. Earlier collaborative studies in cluded a gloss enamel, a flat wall paint, a gloss house enamel, an industrial baking enamel, an interior latex paint, and an exterior latex paint. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2, Referenced Documents 2.1 ASTM Standards: D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products2 D 2369 Test Method for Volatile Content of Coatings2 D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 D 3980 Practice for Interlaboratory Testing of Paint and Related Materials2 3, Summary of Test Method 3.1 The weight and volume of a, stainless steel disk are determined. After the disk is coated with the material being tested, the weight and volume of the disk plus dried coating is determined by weighing in air and then by weighing in a liquid of known density, the volume being equal to the quotient of the weight loss of the coated disk (due to the Archimedes buoyancy effect) divided by the density of the liquid displaced. The liquid may be water, organic liquid such as low-solvency mineral spirits or kerosine, or with special modifications not covered specifically in this method, mercury. The choice of liquid depends upon the nature of the coating tested. 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint wd Related Coatings and Materials and is the direct responsibility of Subcomoittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved April 25, 1986. Published June 1'986. Originally Published as D 2697 - 68. Last previous edition D 2697 - 73 (1979), 2 Annual Book ofASTM Standards, Volume 06.01. N' 1--Distilled water is suitable for most paints. Exceptions are coatings that contain ingredients that are readily leached out of the dry film by the water and low-gloss coatings, the surface of which is poorly wet by water even with surfactant added. (Note 2) Low-solvency hydrocarbon solvent (KB below 36) is also practical for most paints and is preferred by some workers.3 It is considered to be particularly good for paint films not readily wet by water. Analogously, organic solvents must not be used if the coating to be tested contains ingredients that will be dissolved readily by the solvent Lacquers containing monomeric plasticizers would be examples where hydrocarbon solvents should definitely not be used. Coatings formulated much above the CPVC present a special problem, where mercury might be the desired "sus pending" liquid (Note 3), and for solvent-reducible paints hydrocarbon solvent might be considered the poorest (unless it is the objective to obtain values closer to "theoretical" spaces between pigment particles not filled with binder, becoming partially filled with solvent during the test). Note 2--Concentration of surfactant must be kept very low or literature values for the density of the water cannot be used. Note 3--Details of the mercury displacement techniques can be found in the literature.4 3.2 From the measured weights and volumes of the disk before and after coating, the weight and volume of the dried coating film are calculated. Based on the density of the liquid coating and the weight percent nonvolatile matter, the volume of the liquid coating deposited on the coated disk is calculated. The volume of the dried coating divided by the volume of liquid coating, multiplied by 100, provides the volume percent nonvolatile matter in the total liquid coating, 4. Significance and Use 4.1 This test method is intended to provide a measure of the volume of dry coating obtainable from a given volume of liquid coating. This value is useful for comparing the coverage (square feet of surface covered at a specified dry film thickness per unit volume) obtainable with different coating products. 4.2 For various reasons the value obtained may not be equal to that predicted from simple additivity of the weights and volumes of the raw materials in a formulation. One reason is that the volume occupied by a solution of resin in solvent may be the same, greater, or less than the total volume of the separate ingredients: such contraction or expansion in resin solutions is governed by a number of factors, one of which is the extent and direction of spread 3 Bissey, J. E., Official Digest, Federation of Paint and Varnish Production Clubs, Vol 35, 1963, p. 1072, and Ashton, H. E., Materials Research and Standards, Vol l, 1961, p. 549. * Cole, R. J., Journal, Oil Colour Chemists' Assn., Vol. 45, 1962, p. 776. DUP050297544  D2697 between solubility parameters of the resin and solvent, 4.3 The spatial configuration of the pigment particles and the degree to which the spaces between the pigment particles are filled with the binder also affect the volume of a dry coating formulation. Above the critical pigment volume concentration, the apparent volume of the dry film is significantly greater than theoretical due to the increase in unfilled voids between pigment particles. The use of volume nonvolatile matter values in such instances should be care fully considered as the increased volume is largely due to air trapped in these voids. 5. Apparatus 5.1 Analytical Balance. 5.2 Steel Disk, preferably stainless steel, 23/s in. (60 mm) in diameter and 22 gage (0.65 mm) in thickness with a small hole near the circumference. A fine wire, such as Chromel A, 28 gage (0.32 mm), is attached through the hole and made the appropriate length for subsequent suspension of the disk in a liquid. The wire should have a small loop on the upper end so the disk and wire can be hung by this loop on the? balance. N' 4--Instead of steel disks, some analysts use aluminum tubes. In the round-robin results, essentially no difference was found in the precision obtained by both methods. Source and dimensions of these tubes are described in the annex. 5.3 Counterweight, to be placed on the balance stirrup after hanger bow and pan are removed. 5.4 Beaker, 1-L--For-easier manipulation during the weighing of disk in liquid it is advisable to cut the beaker to a height of 4V2 in. (115 mm). 5.5 Support for holding the beaker under the balance stirrup without jamming the pan damper in the floor of the balance. A cork or neoprene ring is suitable when a single-pan balance is used. 5.6 Weight per Gallon Cup, aerometer, or other suitable means for determining the density of the coating material and the suspending liquids if not known. 6. Volume Determination of Uncoated Disks 6.1 Dry the disk in an oven at 110 5C for iO min. Cool and weigh the disk in air. 6.2 Weigh the disk in the liquid to be used for suspension of the coated disk. If water is used as the suspending liquid, a few drops of wetting agent (Note 2) added to the liquid will help to ensure rapid and thorough wetting of the disk. Be careful that no air hubbies form on the disk or wire. Mark the level of liquid in the 1-L beaker necessary for complete immersion of the disk which should be at least % in. (20 mm) above the disk. Maintain this level in subsequent weighings when the disk is coated. 6.3 Record the temperature of the liquid. Obtain the density of the liquid at the temperature used, from a table, such as is found for pure water in Handbook of Chemistry and Physics,s or determine it to 0.001 g/mL. 6.4 Calculate the volume of the disk, G, in millilitres as follows: G -- (w, -- w 2)/D 5 CRC Press, Inc., West Palm Beach, FL, 19S6. where: w{ -- weight of disk in air, g w2 = weight of disk in liquid, g, and D = density of liquid at temperature of test, g/mL. 7. Procedure 7.1 Take a representative sample of the liquid coating ia accordance with Practice D 3925. Mix thoroughly before taking specimens for the individual tests. I 7.2 Determine the weight nonvolatile of the liquid coating 1 by drying 1 h at 110 5C in accordance with Test Method f D 2369. I N' 5--If this method does not apply, then the method used if should be agreed upon between producer and user. K 7.3 Determine to 0.001 g/mL the density of the liquid I coating in accordance with Test Method D 1475. 1 7.4 Dip the disk in the liquid coating and allow the liquid 1 to come up on the wire a distance from `A to lh in. (5 to 15 mm). Allow about 10 min for draining, and blot the coating ft material off the bottom edge of the disk so that beads or 1 drops do not dry on the bottom edge of the disk. I N' 6--In some cases the paint or varnish may be of such 1 consistency that the amount of solid matter remaining on the disk after i dxying is too small for an accurate volume determination. The use of a 1 flat pan with a sidewall about 10 mm in height in place of the disk 1 enables the operator to obtain a more desirable volume of solid matter. ; | However, extra care must be observed to prevent trapping of air at the ; f point where the sidewall meets the bottom ofthe pan. In no case should | bubbles be allowed to be present in cast films. This procedure has not ( been evaluated and no precision statement is available. f 7.5 When beads or drips stop forming, hang the disk in I the oven for 1 h at 110"C (Note 5). Remove and cool. Weigh t the coated disk in air. [ 7.6 Weigh the coated disk in the chosen medium in the ` same manner as for the uncoated disk, recording the | temperature of the liquid at the time of the test. f 8. Calculations 8.1 Calculate the volume of the coated disk, H, in millilitres, as follows: H = (w3 - w^/D where: w3 = weight of coated disk in air, g, w4 = weight of coated disk in liquid, g, and D ~ density of liquid at temperature of test. 8.2 Calculate the volume of the dried coating, F, in millilitres, asfollows: F-- H-- G | j [ i | I I 8.3 Calculate the volume of wet coating, V, in millilitres, from whichthedried coating was obtained, as follows: (w3-wj/(wx P) where: w = nonvolatile matter in 1 g of wet coating, g, and p = density of liquid coating materiaL 8.4 Calculate the percent volume nonvolatile content in a liquid coating as follows: (F/V) X 100 N' 7--The displacement liquid used should be reported with volume percent nonvolatile results. The method of drying the films should also be stated if different from that specified. j ! \ | ' | f r c t V t< d f. ' d1 r f F li n 364 DUP0502 97545 ngin 'efore sting ^thod l used iquid iquid to 15 ating ds or 7 such k after seofa e disk naner. at the ihould as not sk in Veigh n the ; the i, in D 2697 j precision6 9.1 Precision (In accordance with Practice D 3980)--In an ttterlaboratory study of this test method in which one '^fator in each of five laboratories analyzed in duplicate on days four coatings (two solvent-reducible and two #ater-reducible) with nonvolatile contents ranging from 24 0 35 volume %, the pooled within-laboratory standard aviation was found to be 0.444 % with 17 degrees of ^om (DF) and the pooled between-laboratories standard deviation 1.195% with 16 DF, after discarding one day's fgsults from two laboratories on one sample, one day's jesults from one laboratory on another sample, and one 6 Supporting data are available from ASTM Headquarters. Request ^DOl-1052. duplicate result from one laboratory on a third sample. Based on these standard deviations the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 9.1.1 Repeatability--Two results, each the mean of dupli cates, obtained by the same operator on different days should be considered suspect if they differ by more than 1.32 % absolute at volume nonvolatile contents of 24 to 35 %. 9.1.2 Reproducibility--Two results, each the mean of duplicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 3.59 % absolute at the same levels. 9.2 Bias--Bias has not been determined. 10. Keywords 10.1 volume nonvolatile content ANNEX Nonmandatory Information Al. Aluminum Tubes A 1.1 Aluminum tubes,7 uncoated, plain with no cap or liner, #16 neck and orifice, l'A by 6'A in., (32 mm by 160 mm). 7 Tubes manufactured by Teledyne; 2290 W. Townsend St., Chester, PA 19016, have been found satisfactory for this purpose. A 1.2 Cut two 3-in. (75 mm) lengths of tube from the aluminum tubing. Make a sA-in. (20 mm) cut on the flattened end of the tube about `A in. (6 mm) from the end. Slip the tube over a short length of 1 in. (25 mm) inside diameter electrical conduit and return the tube to a round condition. Remove the tube from the pipe and press 1 in. wide strip at an end of the tube toward the center to serve as a hangar attachment. TheAmerican Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of suoh rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ,m litres, .tin a i with ; films 365 DUPO 50297 546 (JjJlM Designation: D 2698 - 90 Standard Test Method for Determination of the Pigment Content of Solvent-Reducible Paints by High-Speed Centrifuging1 This standard is issued under the fixed designation D 2698; the number immediately following the designation indicates the year of original adoption or, in the ease of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense to replace Methods 4022, 4032. 4052 ofFederal Test Method Standard No. 141. Consult the DoD Index ofSpecifications end Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. [ oper I abso they r 9. I react appr abso ! 9. 1. Scope 1.1 This test method covers the separation of pigment from solvent-type paints and the calculation of the percent pigment from the results of nonvolatile determinations on the total paint and the separated vehicle. N' 1--This test method has been proven to be applicable to most , solvent-type paints, the exception being those paints containing severely bleeding pigments or pigments such as carbon black that are very difficult or impossible to centrifuge. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D2369 Test Method for Volatile Content of Coatings2 3. Significance and Use 3.1 This test method describes a rapid method for sepa rating pigment from solvent-reducible paints. 3.2 This test method is used by paint producers and consumers for product acceptance and process control. 4. Apparatus 4.1 Laboratory Centrifuge, capable of developing 32 000 g or higher.3 * 5. Procedure 5.1 Shake the sample for 10 min on a mechanical shaker, stir with a paddle to loosen any caked pigment, and shake again for 10 min. If necessary, repeat until there are no lumps present and the sample is thoroughly mixed. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 25, 1990. Published July 1990. Originally published as D 2698 - 68- Last previous edition D 2698 - 73 (1984)U. 2 Annual Book ofASTM Standards, Vol 06.01. 3 A Sharpies supercentrifuge or an International centrifuge equipped with a high-speed head have been found satisfactory for this purpose. Any centrifuge capable of developing 32 000 g and having facilities for sealing the specimen to prevent solvent loss should also prove to be satisfactory. To calculate the gravities developed by a particular centrifuge use the following calculation: g= rotating radius, cm x r/min2 x 1.118 x 10"5 5.2 Add the mixed paint to the centrifuge container until sufficient paint is added to permit the recovery of 25 ml minimum of clear vehicle. Revolve the bowl at 32 000 g or higher for 15 min or until a clear vehicle is obtained. 5.3 Transfer the vehicle carefully, so as not to dislodge any of the pigment from the walls, into a jar that is immediately capped to prevent any solvent losses by evapo ration. Use this vehicle for the determination of the nonvolatile content of the separated vehicle. i ; j 6. Percent Paint and Vehicle Solids 6.1 Determine the percent nonvolatile content of the original paint and the separated vehicle in accordance with i Test Method D 2369. 7. Calculation | 7.1 Calculate the weight percent pigment of paint, P, as follows: P = (A -B)x 100/100 -- B where: A -- nonvolatile content of paint, %, and B = nonvolatile content of separated vehicle, %. 8. Recovery of Pigment for Analysis 8.1 The pigment may be completely recovered from the centrifuge bowl and washed to remove residual vehicle. This may be done either by a Soxhlet extraction or washing the pigment with a suitable solvent and recentrifuging. N' 2--It has been noted that the removal ofthe pigment from the bowl of a Sharpies supercentrifuge can be facilitated by lining the bowl with a piece of polyester film prior to adding the sample and subse quentlyjust slipping the polyester film along with the pigment out ofthe bowl. I i 9. Precision and Bias 9.1 Precision--The precision estimates are based on an interiaboratory study of this test method in which air drying materials were analyzed in duplicate or triplicate. The following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 9.1.1 Repeatability--The difference between two results, each the mean of duplicate determinations obtained by the same operator, will approximate 0.1 % absolute. Two such values should be considered suspect if they differ by more than 0.25 % absolute. 9.1.2 Reproducibility--The difference between two re sults, each the mean of duplicate determinations obtained by | I f | 1 366 r r DUP050297547 iner until )f 25 mL 000 g or id. ' dislodge r that is t v evapoe nonvol- [tors in different laboratories, will approximate 0.25 % ^0lute. Two such values should be considered suspect if differ by more than 0.5 % absolute. th^ 91.3 This precision pertains to air-drying materials. Heat- active vehicles will have a repeatability and reproducibility ^pfoximately twice as large, that is, 0.5% and 1.0% absolute ly 1.4 It should be noted that when the solvent content of the total paint is very low (15 % or less) the precision of this test method will not be satisfactory unless the nonvolatile determination is precise to the second decimal place. 9.2 Bias--Bias has not been determined for this test method. 10. Keywords 10.1 high speed centrifuging; pigment content; solventreducible paint The American Society lor Testing and Materials takes no position respecting the validity ol any patent rights asserted in connection with arty Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapprovad or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. it of the mce with int, P, as from the Tie. This ring the from the the bowl id subseout of the ed on an rir drying ate. The eptability o results, ed by the Two such by more two re tained by 367 DUP050297548 ( Designation: D 2743 - 68 (Reapproved 1987) adulterate teadjly^ Standard Practices for Uniformity of Traffic Paint Vehicle Solids by Spectroscopy 4.4 Me. prepared 1 from the and Gas Chromatography1 differences either gros This standard is issued under the fixed designation D 2743; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision, A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval with extra) evident by 4.5 Met analysis of 1. Scope 1.1 These practices provide general information on the instrumental techniques available for detecting adulteration or nonuniformity of the chemical nature of the vehicle solids in purchased lots of traffic paints by means of the individual or combined use of infrared and ultraviolet spectroscopy and Method C--Gas Chromatographic Analysis of Oils and Oil Adds Separated from Vehicle Solids.................................. Method D--Ultraviolet Spectral Analysis of Total Vehicle Solids ................................................................................ 16 to 18 19to2i 1.6 This standard may involve hazardous materials, oper. ations, and equipment. This standard does not purport t0 address all ofthe safety problems associated with its use. it # ) spectral gr; 0 detect u the referen cated adult he readily ( an altemat gas chromatography. The procedures given are applicable when traffic paint is selected and purchased on the basis of pre-qualification laboratory or road performance tests, or both, and a reference sample of the original paint so evaluated and selected is retained and compared with test samples representative of subsequent purchased and deliv ered lots of such paint and which are required to be the same as the original reference sample. 1.2 Although not specifically provided for in these prac tices, the methods given may also be applied, with appro priate modification, to evaluating the acceptability of traffic paints that have been purchased on the basis of composition specifications. In such cases, application is limited to the vehicle solids as before, as well as the availability of a suitable standard or range of standards representative of the vehicle solids that are acceptable and with which samples of subse quent delivered lots will be compared. 1.3 The techniques provided are wholly adequate for detecting gross adulteration of the vehicle solids where completely different drying oils, resins, or polymers, or the responsibility-of the user of this standard to establish appropriate safety and health practices and determine tl,ie applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1259 Test Methods for Nonvolatile Content of Resin Solutions2 D1397 Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions2 D2245 Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints3 D2372 Method of Separation of Vehicle from Solvent- Reducible Paints4 D2621 Test Method for Infrared Identification of Vehicle Solids from Solvent-Reducible Paints4 E 105 Recommended Practice for Probability Sampling of Materials5 E 131 Definitions of Terms and Symbols Relating to Molecular Spectroscopy6 5. Selectio 5.1 AH between th test sample It is not po as a guide ence is trul; a moderate evident in t in the ratio the referen judgment n to refer to p in order to nature of th be causing t 5.2 Meth procedures; nonuniform ences from combinations of these have been substituted for those originally contained in the reference sample. In cases of 3. Terminology indication c other methi lesser adulteration or modification, these methods have been 3.1 For definitions of terms and symbols, refer to Defini is sufficient found adequate for detecting vehicle solids, adulterations, or tions E 131. vehicle solk modifications as low as 5 weight % of the vehicle solids. 1.4 These techniques have been developed on the basis of 4. Summary of Methods cant spectra sample is cc cooperative work with alkyd, chlorinated rubber-alkyd, and 4.1 Each of the methods given requires both a reference drying oil, p poly(vinyl toluene) type paints involving the detection of and a test sample of traffic paint and a preliminary separa addition of nonuniformity when such extraneous materials as rosin, fish tion and removal of the pigment component in each. resins, and r oil, hydrocarbon resin, and chlorinated paraffin have been 4.2 Method A involves infrared spectral analysis of cast characteristic added. The procedures given may be, but are not necessarily films of the total vehicle solids to detect spectral differences cases it is b completely applicable to all other types of vehicle solids or between the reference and test samples caused by gross or Methods B a extraneous additions, or both. minor adulteration of the test sample. 5.3 Methe 1.5 The methods provided appear in the following order: 4.3 Method B involves infrared spectral analysis of cast unsaponifiab Method A--Infrared Spectral Analysis of Total Vebicle Solids. Method B--Infrared Spectral Analysis of Unsaponifiable Matter from Vehicle Solids................................................ Section 10 to 12 13 to 15 films of the unsaponifiable matter that has been separated that has eset from the vehicle solids in order to detect spectral differences adulterant m between the reference and test samples caused by less#' i strong spectr; f the vehicl Preting spea: 1 These recommended practices arc under jurisdiction of ASTM Committee CM on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO!.44 on Traffic Coatings. Current edition approved Aug. 15, 1968. Published October 1968. 2 Annual Book ofASTM Standards, Vol 06.02. -3 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 14.02. 6 Annual Book ofASTM Standards, Vol 14.01. Deus conclu ^use its sp differences ( ' l'n, failure t< 368 DU P0502 97549 # D 2743 16 to 18 19 to 21 rials, oper. Purport to its use. It is 'o establish ermine the it of Resin ;r in Alkyd )il Acids in m Solventof Vehicle ampling of delating to to Defini- reference ary separaach. /sis of cast differences }y gross or /sis of cast i separated differences 1 by lesser i iterations of an unsaponifiable nature and which was not * dity evident when using Method A. ^4 Method C involves gas chromatographic analysis of pared methyl esters of the separated fatty acids obtained PG the vehicle solids in order to detea chromatographic Terences between the reference and test samples caused by iher gross or lesser adulteration of the drying oil fraction % extraneous drying oils which may not have been readily 'ient by the use of Methods A and B. 45 Method D involves quantitative ultraviolet spectral aiysis of the total vehicle solids dissolved in a nonaromatic grade solvent to give precise concentrations in order detect ultraviolet spectral absorbance differences between ' jgference and test samples caused by minor or sophistiadulterations of the vehicle solids and which may not ( readily detected by Method A. Method D is to be used as * alternative to Methods B and C. j Selection of Test Methods and Significance and Use 5.1 All of the methods provided involve comparisons 'tween the spectra or chromatograms of the reference and (est samples to determine if they show significant differences. It is not possible at this time to establish quantitative limits js a guide to whether a spectral or chromatographic differ ence is truly significant. Certainly the presence or absence of a moderate or strong peak in the test sample which is not evident in the reference is significant. A persistent difference in the ratios of two peaks of one spectrum as compared to [he reference sample is significant. On the whole, some judgment must be exercised in this respect and it is advisable io refer to published data on infrared or gas chromatography ia order to establish, where feasible, the possible overall nature of the adulterant or its functional group which might be causing the comparison spectra to differ. 5.2 Method A is rapid and the most convenient of the procedures given. It should be utilized first in order to detect nonuniformity of the test sample. Significant spectral differ ences from that of the reference sample can be taken as an indication of adulteration and in such cases the use of the other methods is not necessary. As a general rule. Method A is sufficient to detect gross or major adulteration of the vehicle solids. However, where Method A shows no signifi cant spectral differences, it cannot be assumed that the test sample is completely acceptable since changes in the type of drying oil, polyol, and certain dibasic adds in alkyd resins, addition of certain aliphatic or nonfunctional hydrocarbon resins, and many minor adulterations may not always show characteristic infrared spectral differences. Therefore, in such cases it is best to proceed to additional tests as given in Methods B and C or else alternatively directly to Method D. 5.3 Method B is useful in detecting adulterations that are ^saponifiable or else have an unsaponifiable component that has escaped deteaion in Method A only because the adulterant may have been small in amount and therefore its strong spectral peaks may have been masked over by the rest of the vehicle solids. Some care should be taken in inter preting spectral differences in Method B to avoid an errotcous conclusion that the test sample is unacceptable be muse its spectrum is different. Apparent but unreal differences can occur as a result of incomplete saponificahn, failure to remove all saponifiable material, and varying degrees of contamination of the unsaponifiable fraction with sterols, etc., present in the vehicle solids. After it has thus been firmly established that a real spectral difference does exist, further tests are unnecessary, except that it is wise to resort again to the published literature on infrared to attempt to identify the possible nature of the adulterant. Where Methods A and B indicate acceptability of the test sample, it is still not always possible to rule out adulteration caused by changes or modifications in the saponifiable portion, that is, the type of fatty acid, dibasic acids, and polyol. In such cases, it is best to continue on to Method C for determination of the oil acids, and to other gas chromatographic methods for the polyol and dibasic acids when such equipment is available. 5.4 Method C is extremely sensitive in detecting adultera tions and changes that have been made in the oil or fatty acid portion of the vehicle solids. It can, for example, detect whether linseed, coconut, oiticica, etc., has been substituted for soya oil and vice versa, or whether fish or tall oil has partially or wholly replaced some other drying oil, etc. Consequently, when the results of Methods A and B suggest that the test sample is acceptable and where a drying oil component is known to be present, Method C should be used additionally for more complete assurance of produa uniformity. Where the results from Method C along with those from Methods A and B indicate product uniformity, it is a fairly safe assumption that the product has not been significantly altered. 5.5 Method D is intended as an alternative to Methods B and C and where the results from Method A indicate apparent product acceptability. Method D, by the use of quantitative ultraviolet spectral absorbance data, is an ex tremely sensitive procedure for the detection of complete or even partial adulteration of the test sample. However, considerable caution must be exercised in the preliminary pre-drying of the vehicle solids since it is at this stage that the components are extremely sensitive to oxidative changes. Even minor oxidative changes can seriously affect the absorbance data obtained in ultraviolet spectral analysis and may give an impression that the two samples being com pared are different when in fact they are the same. When these considerations are provided for, and the comparison spectra are identical in Method D as well as in Method A, then it can be assumed that the sample is acceptable. Significant differences in the spectra from Method D would indicate nonuniformity of the product even though Method A may fail to reveal such nonuniformity. 6. Reference Sample 6.1 The reference sample of traffic paint should be at least '/i pt (250 mL) and should be truly representative of the initial paint found acceptable in pre-qualification laboratory or field service tests, or both, and which paint is subsequently specified for purchase. 6.2 In cases where paint is purchased on the basis of formulation specifications and it is desired to utilize these procedures to detect adulteration in delivered lots of paint, reference samples may be synthetically prepared to represent the extremes of the range that will be permitted in the formulation. 369 DUP050297550 D 2743 7. Test Sample 7.1 The test samples of the traffic paint should be at least Vi pt (250 mL) and should be representative ofeach delivered lot of paint that was specified for purchase and which is intended to be the same as the initial reference paint used in the pre-qualifications acceptance tests from which a refer ence sample was retained. 8. Sampling Reference and Test Samples 8.1 Test and reference samples of the traffic paint should be obtained in accordance with Recommended Practice E 105. 9. Preparation of Samples 9.1 Separate the vehicle from the pigment by centrifuging the paint in accordance with Method D 2372. Transfer and preserve the vehicle in a well-stoppered amber bottle. METHOD A--INFRARED SPECTRAL ANALYSIS OF TOTAL VEHICLE SOLIDS 10. Apparatus ~ 10.1 Infrared Spectrophotometer, recording double-beam, and accessory equipment as described in Test Method D2621. 11. Procedure 11.1 Obtain the infrared spectra of a cast film of the vehicle solids of both the test and reference samples by utilizing the procedure referred to in 10.1. In all cases, however, the spectral intensity of both samples should be well matched (by adjusting the film thickness) to within 5 % transmission of each other at the strongest peak, and the transmission of this peak shall be between 5 and' 15 %. It is also desirable to obtain additional spectra on thicker films or else ordinate scale expansion if available, to bring out spectral differences in the weak to moderate peak areas. Here again, the same degree of care should be taken as above to match the film thickness and thereby the overall spectral intensities of the two samples. If desired, an aid in compar ison is to run the test sample against the reference sample in the reference beam in order to show significant differences by means of a single differential spectrum. Considerable caution is required in the use and interpretation of differential spectra as well as proper adjustments ofgain, speed, and slit programs. 12. Interpretation of Results 12.1 Compare the companion spectra from the test and reference samples for identity by visual inspection preferably over a light box. Note particularly the presence- of an extraneous peak or peaks in one which is (arc) not in the other. Also note the ratio of intensities pf two adjacent or pairs of peaks on one spectra and determine whether this ratio is similar on the comparison spectra. Any significant difference should be considered as an indication of lack of uniformity between the reference and test samples. Attempt to ascribe this difference to some extraneous component or formulation difference between the comparison samples by referring to available infrared literature and published spectra. Where it is evident that the comparison spectra are significantly different, no further tests are necessary. When the spectra are identical, proceed to Methods B and C alternatively to Method D for a fuller evaluation of possible' minor or more sophisticated adulteration. METHOD B--INFRARED SPECTRAL ANALYSIS OF UNSAPONIFIABLE MATTER FROM VEHICLE SOLIDS 13. Apparatus 13.1 Same as in 10.1. 14. Procedure 14.1 Treat a portion of the separated vehicle from botl the sample and reference paints so as to obtain an ethec solution of the unsaponifiable matter in accordance with; Test Method D 1397. Take care to ensure rigorous quantita tive separations and similar handling and exposure of 1 comparison samples. Determine the percentage of unsaponifiable matter. Obtain infrared spectra of cast film' of the dried unsaponifiable matter in a manner similar tft that described in 11.1. r 15. Interpretation of Results 15.1 Compare the percentages of unsaponifiable matter Compare the Spectra and interpret the results in a sin manner as in 12.1. Care should be taken to avoid erroneous conclusion that the materials are different when \ fact they are the same. Such a misinterpretation could" caused by incomplete removal of oil acids and varyL degrees of sterol contamination, solvent residues, etc. If it ' firmly established that the companion samples are trul different, then further tests are unnecessary. If, on the oth . hand, the spectra and unsaponifiable contents are identical and the results from Method A were similar, then proceed Method C to determine adulteration of the oil fraction or I oils if such is present or suspected of being present. METHOD C--GAS CHROMATOGRAPHIC ANALYSIS OF OILS AND OIL ACIDS SEPARATED FROM VEHICLE SOLIDS 16. Apparatus and Reagents 16.1 Same as in Method D 2245, 17. Procedure 17.1 Proceed as in Method D2245 utilizing a portion o the, vehicles separated from both the test and refere samples, .t K- 18. Interpretation of Results 18.1 Compare the two recorded chromatograms and th calculated percentages of individual fatty acids for similarity Note particularly the absence or presence of extraneo peaks in one and not the other as well as the percentages individual fatty acids and polymers in one. sample 370 DUP050297551 D 2743 i and c 0r of Possible 1F ; spared to the other. Any significant difference should be 4,eQ as an indication oftest sample adulteration or lack of J^formity. 5IS OF SOLIDS METHOD " -- G < G ' '( G G < E TOTAL VEHICLE SOLIDS |9. Apparatus 19.1 Spectrophotometer, recording double-beam, suitable for use in the ultraviolet region of the electromagnetic spectrum from 190 to 350 nm. from both n an ether lance with is quantitasure of the entage of f cast films similar to ble matter. 1 a similar avoid an nt when in i could be id varying etc. If it is ; are truly l the other e identical proceed to ction or by it. LYSIS 20. Procedure 20.1 On a portion of the previously separated vehicles of the test and reference samples, determine the nonvolatile content by means of Test Method D 1259. On the basis of Oiis determination, quantitatively weigh out, by difference, from the stoppered bottles of the total vehicle, samples to yield 0.2 0.0005 g of vehicle solids and place in a 100-mL beaker. Take care to avoid weighing errors caused ( by evaporation of solvent in the stoppered bottle during*'the weighing process. 20.2 Evaporate the volatile material by placing the beaker over an even heat source maintained at 60 to 65C and under a constant blanket of dry, inert gas, preferably nitrogen, fed through a bell jar in which the beaker is placed. The bell jar should also be fitted with a stoppered separatory funnel with its delivery tube directly over the beaker. Evaporate until all the solvent is completely removed but avoid excessive exposure to these conditions much beyond this point. With the inert gas flow uninterrupted, transfer about 25 to 30 mL of spectral grade cyclohexane to the beaker through the assembled separatory funnel. Remove the beaker and imme diately stir to dissolve all the solid material in the solvent Quantitatively transfer to a 50-mL volumetric flask and fill to mark with additional spectral solvent. This yields a 0.4 % stock solution (wt/vol) of the vehicle solids in solution. If solution is not complete, try gentle warming or else start over using another suitable spectral grad? nonaromatic solvent with an ultraviolet cut-off point at least as low as 220 or 230 nm. 20.3 With appropriate calibrated pipets or hypodermic syringes, volumetric flask, and the same lot of solvent used before, prepare several dilute quantitative solutions from aliquots of each stock solution that will enable quantitative measurements of all peak heights in the subsequent ultravi olet analysis (Note 1). In all cases, a specific quantitative dilution of the reference sample should be matched by exactly the same dilution of the test sample. For each such matched dilution, use the exact same pipet for the test sample as was used for the reference sample to avoid dilution errors of comparison samples. N ' 1--The concentrations and numbers of dilute solutions neces sary to obtain all the spectral peaks characteristic of a material will vary with the type of vehicle solids under examination. Generally, three dilutions of each stock solution to yield 0.03, 0.01, and 0.005 % solutions should suffice. 20.4 Within 24 h, and after making certain that the dilute solution is perfectly clear and without sediment and insolubles, record the ultraviolet absorbance spectrum of the dilute solution using a 1-cm stoppered quartz cell against the solvent blank in a reference cell. Obtain all absorbance peaks for each material that may occur between 200 and 300 nm. By appropriate use of the various dilutions of each sample, the spectral peaks should be made to fall between 0.3 and 0.8 absorbance unit. In all cases, record the exact absorbance value for each of the peaks for both test and reference samples. For each peak at a specific wavelength, the concen trations used for both the test and reference samples should be identical. It is wise to prepare several replicate standard stock and dilute solutions for each concentration indepen dently ofeach other in order to obtain an idea of the range in each peak absorbance of the standard sample that might be expected in this procedure, especially as a result of the preliminary removal of original solvent by heating and its possible oxidative effects. 21. Interpretation of Results 21.1 Compare the nature and shape of the ultraviolet absorption curves obtained for both the test and reference samples. Any significant difference is an indication of adulteration or nonuniformity. Also compare the absorbance value of each peak given by the test sample with that given by the comparison reference sample. Any significant differ ence should be an indication of adulteration or nonuni formity. It is difficult to fix precise criteria for spectral differences that apply to all materials. As a general guide, the following criteria may be useful for evaluating comparable absorbance peaks. Comparison peaks should be within 0.05 absorbance units when occurring between 220 and 350 nm, and within 0.08 at lower wavelengths. 22. Report 22.1 Indicate uniformity or lack of uniformity of the vehicle solids of the test sample with respect to the reference sample and the method or methods (A, B, C, and D) used for this judgment. If possible, attempt to report the nature of possible adulterant(s) present or the cause of the nonuni formity. portion of . reference The American Society for Testingand- Materials takes no position respecting the velidity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly edvised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, ere entirely their own responsibility. ns and the similarity, extraneous :entages of sample as This standardis subject to revision at any time by the responsible technical committee andmust be reviewedevery live years and If not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or lot; additional standards and should be addressed to ASTM Headqaarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may abend. If you feel that.your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1915 Race St., Philadelphia, PA 19103. 371 DUPO50297552 Designation: D 2792 - 69 (Reapproved 1987) Standard Test Method for Solvent and Fuel Resistance of Traffic Paint1 This standard is issued under the fixed designation D 2792; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval, A superscript epsiloa (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method describes a laboratory test for determining the resistance of a dried film of traffic paint to the action of a specified hydrocarbon solvent or gasoline fuel test fluid. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D471 Test Method for Rubber Property--Effect of Liquids12 2.2 Federal Standard: TT-S-735 Standard Test Fluids for Hydrocarbons3 3. Summary of Method 3.1 The test paint is applied to a specified, properly prepared, tin panel. After aging, the coated panel is im mersed in the hydrocarbon test fluid for a specified period of time at a specified temperature. The paint is examined for blistering, wrinkling, and loss of adhesion immediately upon removal and for complete hardness after a specified recovery time. 4. Significance and Use 4.1 Traffic paints must have good resistance to motor oil and fuel drippings on the highway. This test method de scribes the procedure necessary to measure the resistance of traffic paint to reference test fluids in order to simulate this type of action. 5. Apparatus 5.1 Tin Panel--Panels shall be cut from bright tin plate weighing not more than 25 g and not less than 19 g/dm2 (0.51 to 0.39 lb/ft2). The panel should be about 75 by 130 mm (3 by 5 in.). 1 This test method is under the jurisdiction of ASTM Committee D-i on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.44 on Traffic Coatings. Current edition approved Oct. 3, 1969. Published December 1969. 2 Annual Book ofASTM Standards, Vol 09.01. 3 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NFODS. 5.2 Film Applicator, which will produce a 3 or 6-mi] (0.003 or 0.006-in.) (76 or 142-pm) wet film thickness. 6. Reagents and Materials 6.1 Test Liquid--The testing liquid shall be specified by the purchaser and shall be selected from the following dependent on the paint tested: 6.1.1 Type I of Federal Specification TT-S-735 which is the same as ASTM Reference Fuel A {ASTM Test Method D471). 46.1.2 Type III ofFederal Specification TT-S-735 which is the same as ASTM Reference Fuel B (Test Method D 471), 7. Procedure 7.1 Clean the tin panels thoroughly with a suitable solvent, and buff lightly with fine steel wool. Prepare at least 3 panels for each paint to be tested. 7.2 Examine the test paint, remove any skins that are present, stir with a paddle to loosen any settled pigment, and mix thoroughly. 7.3 Draw down the material on the panels using a film applicator that will produce a 3 or 6-mil (76 or 142-p.m) wet film as specified by the purchaser. 7.4 Air dry the coating for the time specified by the purchaser (usually 90 h) and then immerse the panels to hat their length in the test liquid contained in a covered glass beaker at the temperature specified by the purchaser (gen erally 70 to 90F (21 to 32*C)). Use a separate beaker for each paint tested: 7.5 At the end of the specified time (usually 4 to 18 b, depending on the? type of paint) remove the panels and examine immediately for blistering, wrinkling, and loss of adhesion. 7.6' Allow the panels to dry at normal temperatures for the purchaser-specified time (generally 24 h), and examine for film defects and softening in comparison with the unimmersed portion of the panels. 8. Report 8.1 Report whether blistering, wrinkling, or loss of adhe sion is evident immediately upon removal of panel from the test fluid as determined in 7,5. 8.2 Report whether any softening of the film is evident after the panel has recovered as determined in 7.6. 9. Precision 9.1 No statement of precision, in terms of percentages, can be made, although repeatability and reproducibility ate exceptionally good. iM iiiiiia ttiliiiM DU PO50297553 I i or $-m hickness. >e specified bv the following >-735 which is 1 Tet Method 3-735 which is ethod D 471^ a suitable solpare at least 3 skins that are 1 pigment, and j s using a film r 142-jim) wet ecified by the panels to half . covered glass urchaser (gen- jeaker for each \ ! illy 4 to 18 h, e panels and l, and loss of ratures for the 1 examine for >n with the .r loss of adhepanel from the film is evident i n 7.6. ! of percentages, oducibility am \ i D2792 The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited either forrevision of thfs standard or for additional standards and should bo addressed to ASTM Headquarters. Your comments will receive careful consideration af a meeting of the responsible technical committee, which you may attend. It you feet that your commsnts have nof received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 373 DUP050297554 Designation: D 2793 - 69 (Reapproved 1987) Standard Test Method for Block Resistance of Organic Coatings on Wood Substrates1 This standard is issued under the fixed designation D 2793; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision, A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This method covers the determination of the block resistance of organic coatings on wood and wood-based substrates. Block resistance is the ability of a coating to resist sticking to another surface and to resist any change in appearance, when it is pressed against that surface for a prolonged period of time. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Summary of Method 2.1 The coatings to be tested are applied to the desired substrate. They are cured in a manner duplicating the condition of end use as much as possible. Then a stack of these painted substrates is formed and subjected to a specified pressure for a sufficient time to develop any sticking tendencies that exist. The pressure is released and the painted surfaces are examined for any signs of sticking. If blocking (forming a block by panels sticking together) occurs, the material is unsatisfactory. If no sticking or damage to the film surface occurs, the material is satisfac tory. 2.2 When the conditions of production finishing are established and known, the method of application, the substrate, film thickness, and cure of the film should duplicate those conditions as closely as possible. 2.3 When the conditions of storage and shipment are established and known, the temperature, relative humidity, duration, and pressure used for the test should duplicate those conditions as closely as possible. 3. Apparatus 3.1 Rigid Platens, 4-in. (100-mm) square, capable of being maintained at 120 2F (49 TC). 4. Test Specimens 4.1 For those cases where the intended use conditions are not established or known, the following specifications or some set of specifications agreed upon by the purchaser and seller apply: The test coating shall be applied by normal spray, using air, to a 4 by 4-in. (100 by 100-mm) panel. The panel shall be a piece of 'A-in. (6.4-mm) SIS (smooth one 1 This method is under the jurisdiction of ASTM Committee D 1 on Paint and Related Coatings and Materials, Effective Oct. 3, 1969. side) standard hardboard. The dry film thickness of pig. I mented coatings shall be 1.5 0.2 mils (38 5 (am), and of ; clear coatings shall be 1.2 0.2 mils (30 5 jam). Cure of the coating shall be as agreed and should be standardized for ! each coating. N' 1--Film thickness can be measured by weight difference before and after painting, but this requires careful conditioning of the substrate under standard temperature and humidity conditions prior to each weighing. Film thickness can also be determined by using an aluminum tab alongside the test panel and measuring the film thickness with a standard eddy-current gage or using a steel panel with a magnetic film thickness gage. ; 5. Procedure 5.1 After 90 s cooling under ambient conditions or as agreed upon, make a stack of six panels and place under a uniform pressure of 35 2 psi (240 20 kPa) for Class 1,20 j 1 psi (140 10 kPa) for Class II, and 5 `A psi (35 1.7 ' kPa) for Class III. These classes are arbitrary and simply designate three groups of coatings or possibly three groups of end uses. Stack the panels in the following order from the top to the bottom: i {a) Face down. (b) Face down ; (c) Face up. (d) Face down. (e) Facedown. | (/) Face up. This provides for two face-to-face contacts and two face- ; to-back contacts. Apply the load through rigid 4-in. square j (100-mm square) pressure plates. Apply the load for a j minimum of 24 h. Other pressures, types of pressure plates, 1 and times may be used if agreed between the purchaser and ; seller. Conduct the test under ambient conditions but use ; press platens heated to 120 2F (49 1C). Slip sheets : should not be used unless they are known to be used during storage of shipment. N' 2--The most difficult portion of this test method to Stan- dardize on intelligently is the proper pressure to employ. Stacking j pressure in production would be calculated as follows: (DHA\/A2) x F where: D = board density, H = height of stack, A, = area of stack, A2 - area of support, and F = safety factor. The area of support is difficult to establish. In some instances board is | ; j stacked smoothly on the floor while in other instances the stack is ; supported on 2 by 4 or 4 by 4 stringers which cut the support to vei) small ar kPa) are are suita N' with wat high rel. warehou N' water qv when sta 5.2 i pick up then th panels: conside appears 374 DUPO 502 97555 less of pig. pm), and of Cure ofthe iardized for jht difference tioning of the .itions prior to by using an film thickness ith a magnetic itions or as ace under a >r Class I, 20 >si{35 1.7 and simply ee groups of from the top D 2793 sjjail areas. It has been found that pressures of20 to 50 psi (140 to 340 jjpa) are suitable on hardboard substrates while 2 to 5 psi (14 to 35 kPa) jic suitable on solid wood surfaces. No t e 3--Many coatings are plasticized if they are contaminated with water. Ifpossible, therefore, it is advisable to run blocking tests at as jjgh relative humidities as might be encountered in production of warehousing. No t e 4--Blocking tests shall be run with panels wet with water, if water quenching is used for cooling the boards and die boards are wet when stacked in production. 5.2 At the end of the test period remove the pressure and pick up the stack in such a way that first the bottom panel, then the next to the bottom panel, and eventually all of the panels are free to fall of their own weight. This falling free is considered as passing the test if there also is no change in the appearance of the coated surfaces of any of the panels. 6, Report 6.1 This is a go/no-go test for both face-to-face and face-to-back conditions. In addition to the separate state ment of satisfactory or not satisfactory under both of these conditions, the nature of the failure should be reported. The report should also include the particulars of the test as follows: 6.1.1 Type of substrate, 6.1.2 Method of application, 6.1.3 Curing cycle, 6.1.4 Film thickness, 6.1.5 Temperature, humidity, and pressure of the blocking test, 6.1.6 Type of stacking including identification and type of slip sheets if any, and 6.1.7 Duration of test. 7. Precision 7.1A round robin will be made to establish precision. The American Society for Testing and Materials takes nojiosition respecting the validity ofany patent rights asserted !n connection with any item mentioned in this standard. User3 of this stdhdard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if notrevised, either reapproved or withdrawn. Your comments are invited either for revision ofthis Standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. id two face1-in. square load for a sure plates, rchaser and ms but use Slip sheets used during ethod to stanploy. Stacking tances board is es the stack is support to very 375 DUP0502 97556 I Designation: D 2794 - 90 Standard Test Method for Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact)1 2 ] This standard is issued under the fixed designation D 2794; the number immediately following the designation indicates the year of original adoption or, in the ease of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers a procedure for rapidly deforming by impact a coating film and its substrate and for evaluating the effect of such deformation. 1.2 This test method should be restricted to testing in only one laboratory when numerical values are used because of the poor reproducibility of the method. Interlaboratory agreement is improved when ranking is used in place of numerical values. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards; D609 Practice for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 3. Terminology 3.1 Description of Term Specific to This Standard: 3.1.1 impact resistance, of a coating--the number of inch-pounds (kilogram-metres) required to produce cracking in the deformed coating. 4. Summary of Test Method 4.1 The organic coatings under test are applied to suitable thin metal panels. After the coatings have cured, a standard weight is dropped a distance so as to strike an indenter that deforms the coating and the substrate. The indentation can be either an intrusion or an extrusion. By gradually in creasing the distance the weight drops, the point at which failure usually occurs can be determined. Films generally fail by cracking, which is made more visible by the use of a magnifier, by the application of a copper sulfate (CuS04) 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.23 on Physical Properties of Applied Paint Films. Current edition approved July 27, 1990. Published November 1990, Originally published as D 2794 - 69. Last previous edition D 2794 - 84l. 2 Annual Book ofASTM Standards, Vol 06.01. solution on steel, or by the use of a pin hole detector. 5. Significance and Use 5.1 Coatings attached to substrates can exhibit cracking when subjected to rapid deformation, produced by impacts of objects during manufacturing and service. This test method has been very useful in evaluating attached coatings for their ability to resist cracking caused by impacts. | 6. Apparatus 6.1 Tester, consisting of a vertical tube to guide a cylindrical weight that is dropped on a punch resting on the test panel.3 4 6.1.1 Guide Tube, 24 to 48 in. (0.6 to 1.2 m) long mounted f vertically in a base plate. A slot is cut lengthwise on one side S of the tube to act as a guide for a cylindrical weight that fits inside the tube. Graduations are marked in inch-pounds along the slot. The base is constructed so that a thin flat ; panel can be inserted at 2 in. (50 mm) below the tube. | 6.1.2 Weight, metal cylinder, made to fit inside the guide tube. A pin is fitted into one side of the weight to act as a guide by riding in the slot ofthe tube and to serve as a handle by which the weight can be raised and released and serve as the indicator of inch-pounds (kilogram-metres). 6.2 Indenter--A steel punch with a hemispherical head having a diameter of either 0.500 in. (12.7 mm) or 0.625 in. (15.9 mm). The head rests on the test panel and the punch is i held vertically by a guide ring. 6.3 Panel Support--A steel fixture with a 0.64-in. (16.3- mm) diameter cylindrical hole centered under the indenter for supporting the test panel. 6.4 Magnifier. 6.5 Pin Hole Detector,4 7. Reagents 7.1 An acidified copper sulfate (CuS04) solution prepared by dissolving 10 g of CuS04-5H20 in 90 g of 1.0 N hydrochloric acid (HC1). 8. Test Specimens 8.1 Apply uniform coatings ofthe material to be tested to 3 Suitable instruments arc the Gardncr-SPI Modified Impact Tester, available from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910, or the Universal Impact Tester Model No. 172, available from Paul N. Gardner Co., Inc., 316 N.E. First St., PO Box 10688, Pompano Beach, FL 33061-6688. Equivalent apparatus may be used. 4 Suitable instruments are the Elcometer Pinhole Detector Model 104 and Zorelco Model 169 Pin Hole Detector, available from Zorelco Carp., PO Box 25500, Cleveland OH 44125, and the K-D Bird Dog Holiday Detector. 24-gage (0.02 conversin < practice D 6' jrnuni of fou No t e 1--Ti Methods D 823 Other gage ste producer and tl 8.2 Cure t and tempera user. No t e 2--T) accordance wit 9. Condition 9.1 Unless and the user, at 73.5 3..` Conduct the on removal1 10. Procedu 10.1 Insta or agreed up coated side e sure the par indenter is Lightly place tube so that weight up tl failure will c indenter. 10.2 Ren observe the i are evident, creasing 1 i observed, re slightly abo' first trial. T one height; 10.3 Exai the followin 10.3.1 Us 10.3.2 He acidified cc 376 DUP0502 97557 :tor. t cracking >y impacts This test d coatings ts. > guide a ing on the > mounted n one side tit that fits eh-pounds i thin flat tube. the guide o act as a is a handle id serve as rical head r 0.625 in. e punch is in. (16.3indenter prepared of 1.0 N ; tested to ter, available Jilver Spring, tom Paul N. > Beach, Fi del 104 and rp., PO Box D 2794 ;4-gage (0.025 in. or 0.63 mm) steel panels treated with a c0l)version coating in accordance with Procedure A of practice D 609, unless otherwise specified. Prepare a min ium of four coated panels for the material. N' 1--The coatings should be applied in accordance with Test wjthods D 823, or as agreed upon between the producer and the user. Other gage steel panels may be used if agreed upon between the producer and the user. 8.2 Cure the coated panels under conditions of humidity afld temperature agreed upon between the producer and the user- N' 2--The thickness of the dry coatings should be measured in accordance with Test Methods D 1186. 9, Conditioning 9.1 Unless otherwise agreed upon between the producer ppd the user, condition the coated test panels for at least 24 h at 73.5 3.5F (23 2"C) and 50 5 % relative humidity. Conduct the test in the same environment or immediately 0n removal therefrom. jO. Procedure 10.1 Install the punch having the head diameter specified or agreed upon. Place the test panel in the apparatus with the coated side either up or down as specified or agreed upon. Be sure the panel is flat against the base support and that the indenter is in contact with the top surface of the panel. Lightly place the weight on the indenter and adjust the guide tube so that the lifting pin is at the zero mark. Raise the weight up the tube to a height where it is expected that no failure will occur. Release the weight so that it drops on the indenter. 10.2 Remove the test panel from the apparatus and observe the impact area for cracks in the coating. If no cracks are evident, repeat the procedure at a greater height, in creasing 1 in. (25 mm) at a time. Once visible cracks are observed, repeat the test five times at each of three heights; slightly above, slightly below, and at that determined in the first trial. Test in a random fashion so that all impacts from one height are not made in succession or on one panel. 10.3 Examine the impacted areas for cracking by one of the following methods; 10.3.1 Use a magnifier to examine the area for cracks. 10.3.2 Hold a white flannel-type cloth saturated with the acidified copper sulfate (CuS04) solution (7.1) over the impacted areas for at least 15 min. Remove the cloth and examine both the test areas and cloth for. evidence of copper deposition or iron-rust staining respectively. N' 3--The. copper sulfate solution will not perform properly on zinc-phosphate-treated metal unless the conversion coating cracks. 10.3.3 To detect breaks in the film with a pin hole detector, first connect the ground lead from the instrument to the bare substrate and connect the instrument to an electrical power source. Moisten the probe sponge with tap water and slowly draw the probe over the impact area. The presence of cracks will be indicated by an audible alarm. 10.4 For each inch-pound (kilogram-metre) level, tabulate the number of times the coating passed or failed. The value where the results change from mainly passing to mainly failing is the impact failure end point. 11. Report 11.1 Report the following for each coating tested: 11.1.1 The inch-pounds (kilogram-metres) at the impact failure end point, 11.1.2 Whether intrusion or extrusion was used, 11.1.3 Diameter of the punch used, 11.1.4 Thickness of coating, 11.1.5 Substrate thickness and type of metal, 11.1.6 Method of panel preparation, and 11.1.7 Atmospheric conditions under which the coated panels were conditioned and tested. N' 4--Because of the poor reproducibility of this method, the reporting of inch-pounds (kilogram-metres) in comparing coatings for impact resistance should be restricted to one laboratory. For interlabo ratory comparisons, rankings ofcoatings for impact resistance should be reported. 12. Precision 12.1 On the basis of an interlaboratory test in which operators in six laboratories tested three paints having a broad range of impact resistance on two metal substrates, the between-laboratories coefficients of variation were found to be as follows: Brittle coating (less than 6 in.-lb) Average coating (between 6 and 140 in.-lb) Flexible coating (more than 140 in.-lb) (0.625 in.-diameter punch) Coefficient of Variation Intrusion, Extrusion, %% 25 100 80 100 10 25 The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is sub/ect to revision atany time by the responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapproved or withdrawn. Your comments are invitedeither for revision ofthis standard ortor additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have hot received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 371 DUP050297558 Last ASTM Designation: D 2801 - 69 (Reapproved 1981)e1 Standard Test Method for Leveling Characteristics of Paints by Draw-Down Method r#De This method covers the laboratory determination of the relative leveling characteristics of liquid water-reducible 0r solvent-reducible coatings in white and light tints. Formerly under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials, this test method was discontinued in 1990. | Scope : 1.1 This [ the suscept: station off 1.2 This whether fill coating and j 1.3 This | ations, ana address all the respom appropriate applicabilit 2. Referem 2.1 AST B H7 M D609 M ; `i j Paint, D823 T Thickr Test P D1005 1 ness oi D11861 Dry F 1 to a Ft D1400' Dry F plied t [ D1654 Sped: D 1730 minu: E 104 I midit . 2.2 Ink i . !i * ! ISO 462 I . on Stt 3. Summa 'c 3.1 Coa i$ f ----------1 This raetl Related Coatii ! DO 1.27 on Ac Current edi Cpublished as [ ;L ; 2 Annual B 345 Annual Annual Annual B B B 6 Available ) Floor, New Y i i_____ ___________ ._ . . . 378 J .. .. DUP050297559 Designation: D 2803 - 82 (Reapproved 1087J Standard Test Method for Filiform Corrosion Resistance of Organic Coatings on Metai1 This standard is issued under the fixed designation D 2803; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval, superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This method covers two procedures for determining the susceptibility of organic-coated metal substrates to for mation of filiform corrosion. 1.2 This method is limited to the determination of whether filiform corrosion will occur between the organic coating and substrate. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: B 117 Method of Salt Spray (Fog) Testing2 D 609 Methods for Preparation of Steel Panels For Testing Paint, Varnish, Lacquer, and Related Products3 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D 1005 Test Method for Measurement of Dry-Film Thick ness of Organic Coatings Using Micrometers3 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base3 D 1400 Test Method- for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base3 D1654 Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive Environments3 D 1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting4 E 104 Practice for Maintaining Constant Relative Hu midity by Means of Aqueous Solutions5 t 2.2 International Standard: ISO 4623 Paint and Varnishes--Filiform Corrosion. Test on Steel6 3. Summary of Method 3.1 Coated metal specimens are scribed and placed in a 1This method is under the jurisdiction of ASTM Committee D-l on Paint and' Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.27 on Accelerated Tests for Protective Coatings. Current edition approved June 25, 1982. Published September 1982. Originally published as D 2803 - 69 T. Last previous edition. D 2803 - 70{1974). 1 Annual Book ofASTM Standards, Vols 03.02and 06.01. 3 Annual Book ofASTM Standards, Vol 06.01. * Annual Book ofASTM Standards, Vols 02.05 and 06.0K 5 Annual Book ofASTM Standards, Vols 08.03, 10.01, and 11.03. ' 6 Available from American National Standards Institute, 11 W. 42nd St., 13th Floor, New York, NY 10036. corrosive atmosphere to initiate corrosion. The specimens are then exposed to controlled temperature and humidity conditions known to be conducive to filiform corrosion. 3.2 In Procedure A, panels are subjected to a preliminary exposure in the salt spray cabinet to initiate corrosion, rinsed, and placed in a humidity cabinet. In Procedure B, based on ISO 4623, panels are either exposed to salt spray or dipped in a salt solution but not rinsed before placing in the humidity cabinet operated at a higher temperature than in Procedure A. 4. Significance and Use 4.1 Some organic coatings applied to metal substrates exhibit filiform corrosion when there is a break in the coating film and the relative humidity is in the 70 to 95 % range. 4.2 This method can be used to determine the suscepti bility of organic coated metal substrates to the formation of filiform corrosion. 5. Definitions 5.1 filiform corrosion--a special type of corrosion that occurs under coatings on metal substrates that is character ized by a definite threadlike structure and directional growth. Filiform corrosion usually occurs between 70 and 95F (20 and 35C), with a corresponding relative humidity range of 60 to. 95 %; above 95 % humidity, blistering rather than filiform corrosion may occur. 6. Apparatus 6.1 Salt-Spray Chamber as described in Method B 117, for salt-spray (fog) testing. N' 1--The preferred initiator of corrosion at the scribe is the salt-fog atmosphere described in Method B 117. Exposure of the specimens for 2 to 4 h in a closed cabinet to the atmosphere above a 1 % acetic acid solution is an acceptable alternative. 6.2 Humidity Cabinet--Any cabinet with suitable tem perature and humidity controls with air circulation may be used. The size and detailed construction of the apparatus are optional, provided the conditions meet the requirements of this method. 7. Test Specimen 7.t The composition, surface preparation, and number of test specimens shall be agreed upon between the producer and the user. Steel is the preferred substrate, but other metals such as aluminum, copper, and stainless steel may be used. Zinc and 'zinc-coated steel are not recommended because filiform corrosion generally does not occur on zinc. N' .2--Applicable test panel description and surface preparation methods are given in Method D 607 and Practices D 1730. 7.2 Preparation ofTest Specimens--The method ofappli cation, film thickness, curing, and conditioning shall be agreed upon between the producer and user. 379 DUP050297560 # D 2803 N' 3--Test Methods D 823 gives application methods that can be used to produce films of uniform film thickness. N' 4--Test Methods D 1005, D 1186, and D 1400 give proce dures that can be used for measurement of dry film thickness. 7.3 Scribe the test specimen in accordance with Method D 1654 or as agreed upon between the producer and user. 7.4 The back and edges of the panel should be protected with an anti-corrosion coating or tape, unless edge failure is being evaluated. g. Procedure A 8.1 Expose the test specimens to the salt-fog atmosphere in accordance with Method B 117 for at least 4 h and not more than 24 h, or as agreed upon between the producer and user. 8.2 Remove from the salt-fog cabinet and thoroughly rinse with distilled or demineralized water. Do not permit specimens to dry before placing in the humidity cabinet. 8.3 Place the specimens in the humidity cabinet sd they are no closer together than 1.5 in. (40 mm) and not in contact with any metal. Operate the cabinet at 77 3!F (25 2C) and 85 2 % relative humidity unless otherwise agreed upon between the producer and user. N' 5--The recommended means of maintaining the specified relative humidity is to utilize trays of saturated potassium chromate solution (650 g/L). Recommended Practice E 104 describes other methods for maintaining relative humidity, but they may affect the degree and rate of filiform corrosion. 8.4 Inspect the specimens at intervals of approximately 168 h for development of threadlike filaments from the scribe. Exercise care to maintain wetness of specimens during inspection, since drying stops the original pattern of filiform corrosion. New filiform, may develop on continued exposure but at different points. 8.4.1 Filiform corrosion will be noted as threadlike fila ments (see Note 6), initiating at the scribe. A standard method of rating failure due to filiform is not available. The uniformity of filament growth in direction, width, height and frequency precludes a precise rating system. Photographs of filiform failure are preferred for recording test results. Otherwise, a brief description of the filament growth and their frequency can be made. N' 6--The nature of grinding and grain direction on panels can influence the direction of filiform growth. 8.5 The normal test period is 6 weeks (1008 h). Other periods may be used at the option of the producer and user. 9. Procedure (ISO 4623) 9.1 Two alternative initiations of corrosion are available, based on initiation by dipping in sodium chloride solution (see Note 7) or exposure to salt fog. The dipping technique is generally preferable for air drying and low-durability mate- rials. For high-durability systems such as automotive finishes applied to phosphated steel, the dipping technique may not produce filiform corrosion and. for these systems, it is preferable to adopt the salt-fog technique. In such cases, the necessary period of exposure to salt fog depends on the durability ofthe material under test but should rarely need to exceed 24 h. N' 7--Sodium chloride 0.1 % (w/v) solution (for dipping tech nique] is prepared by dissolving 1 g of reagent grade sodium chloride (NaCI) in 1 L ofdistilled or demineralized water. Place this solution in a vessel suitable for complete immersion of the test panel 9.2 Dipping Technique: 9.2.1 Immerse the scribed specimen for 30 to 60 s in the sodium chloride solution (see Note 7). 9.2.2 Take the specimen out of the solution and remove any drops of liquid adhering to it, taking care not to remove the solution from the scribed marks. 9.2.3 Place .the specimen in a humidity cabinet main tained at 104 3.5F (40 2C) and 80 5 % relative humidity. 9.2.4 Repeat the immersion procedure every 3 or 4 days until the end of the test cycle (21 days) or as agreed upon between the producer and the user. 9.3 Salt-Fog Technique: 9.3.1 Expose the scribed test specimen to the salt-fog atmosphere in accordance with Method B 117 for at least 4 h or not more than 24 h or as agreed upon between the producer and the user. 9.3.2 Remove the test specimen from the salt-fog cabinet and remove any drops of liquid adhering to it, taking care not to remove the solution from the scribed marks. 9.3.3 Place the specimen in a humidity cabinet main tained at 104 3.5F (40 2C) and 80 5 % relative humidity for the specified period agreed upon between the producer and the user. 9.4 Follow the procedures in 8.4 and 8.4.1. 10. Report 10.1 The report shall include the following: 10.1.1 Initiation procedure, 10.1.2 Humidity cabinet operating temperature, 10.1.3 Exposure period, and , 10.1.4 Rating of coatings as described in 8.4.1. 11. Precision 1J. 1 Procedure A--Twelve laboratories,, using three types of cofrosion initiations, three coatings and three substrates, were in excellent agreement in their ranking of the suscepti bility to filiform corrosion by this procedure. 11.2 Procedure B--Has been judged reproducible by Working Group 2 of ISO/TC35/SC9. ; i % \ \ f f The American Society tor Testing ant) Materials takes no position respecting the validity otany patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ofany such patent rights, and the risk ot Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewedevery five years and if not revised, eitherreapproved orwithdrawn. Your comments are invitedeither for revision ofthis standard or foradditional standards ' and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If ypujeef that your comments have not received a fair hearing you should make your. views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. i i. re ai W b: 2. a. ti a a n a r 380 DUP0502 97561 toy mate, 'e finishes may not ms, it is cases, the is on the ly need to aping techm chloride >lution in a Designation: D 2805 - 88 Standard Test Method for Hiding Power of Paints by Reflectometry1 This standard is issued under the fixed designation D 2805; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. INTRODUCTION D s in the i remove 0 remove et main1 relative or 4 days ;ed upon : salt-fog .least 4 h ween the g cabinet ring care et main) relative ween the ee types lbstrates, suscepticible by Using equations deprived from Kubelka-Munk turbid media theory (1-4)2, the reflectance of a coating can be predicted for any film thickness from measurements made at only one. On this basis several easy and accurate test methods (5,7) have been developed for determining hiding power. In the past such test methods have been considered difficult due to complexities, apparent and actual, in the treatment of data. The present test method has been simplified in this respect, primarily by adapting it fully for computer calculations. Although the use of broad-band reflectometry makes this test method theoretically valid only for nonchromatic (white or gray) colors, good agreement has been obtained with chromatic paints as well. This is undoubtedly because the experimental measurements are made fairly close to the hiding power end point so that the Kubelka-Munk extrapolation and thus any associated error is relatively small. This test method is therefore recommended without restriction as to color. 1. Scope 1.1 This test method covers the determination, without reference to a material paint standard, of the hiding power of air dry coatings with Y tristimulus values greater than 15 %. With appropriate modification, it can also be used to test baking finishes. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts3 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products3 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates3 D3924 Specification for Standard Environment for Con ditioning and Testing Paint, Varnish, Lacquer, and Related Materials3 1 This test method is under the jurisdiction ofASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO1.26 on Optical Properties. . Current edition approved March 25, 1988. Published May 1988. Originally published as D 2805 - 69 T, Last previous edition D 2805 -85. 2 The boldface numbers in parentheses refer to the list of references at the end \ of this standard. 3 Annual Book ofASTM Standards, Voi 06.01. E 97 Test Method for Directional Reflectance Factor, 45-deg, 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry4 E 179 Practice for Selection of Geometric Conditions for Measurement of Reflectance and Transmission Proper ties of Materials5 E 284 Definitions of Terms Relating to Appearance of Materials5 3. Terminology 3.1 Definitions--For definitions used in this test method, see Definitions E 284. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 contrast ratio--the ratio of the reflectance of a film on a black substrate to that of an identical film on a white substrate. 3.2.1.1 Cw--the contrast ratio with a white substrate of reflectance W. Thus; Ciy -- 3.2.1.2 C--the contrast ratio with a white substrate for which W = 0.80. Thus: C^/Ro.,,0 3.2.2 reflectance--the daylight luminous diffuse reflec tance factor (specular reflection excluded). Also referred to in this test method as the y-tristimulus value. This value may be expressed as a percent or a decimal fraction, the latter being preferred and usually required for mathematical calcu lations. 3.2.2.1 reflectivity, R,,--the reflectance of film thick enough to have the same reflectance over both a black and a white substrate. 4 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 5 Annual Book ofASTM Standards, Vol 14.02. 381 DU PO 502 97562  D 2805 3.2.2.2 Ro--the reflectance of a film on a black surface 6.1.2 Black and White Paper Charts7--The surface shall with a reflectance of 1 % or less, which is effectively zero for be smooth and level, and impervious to paint liquids. The the purpose of this test. black area shall have a maximum reflectance of 1 % and the 3.2.2.3 W--the reflectance of a white substrate. white area a minimum reflectance of76 %. 3.2.2.4 Rn--the reflectance of a film applied on a white 6.2 Balance, accurate to 0.1 mg. substrate of reflectance W. 6.3 Glass Slides8--Round or square plates of thickness 3.2.2.5 .Ro.so--the reflectance of a film applied on a similar to that used for microscope specimen slides, with a substrate having a reflectance of 80 %, which is the standard minimum area of 40 cm2. white-substrate reflectance in paint technology. 6.4 Reflectance-Measuring Instrument--One that allows 3.2.3 scattering coefficient, S--the ability of a material to only diffusely reflected, radiant flux to be incident upon the internally scatter and thereby reflect light; expressed in this measuring element. It shall employ a photometric system, test method in the same units as spreading rate. including source, filters, and receptor, that provides a re 3.2.4 spreading rate, H--film area per unit volume of sponse closely similar to the product of the spectral luminous coating, in this test method expressed in square metres per efficiency function of the CIE standard observer and source litre (m2/L). It is also frequently expressed in square feet per C. It shall provide readings to at least the third decimal place gallon (ft2/gal). 3.2.4.1 spreading rate, Hx--an experimentally deter and permit estimation to the fourth. 6.5 Template,9 with a film area approximately 100 cm2 9 i mined value of H. determined to the nearest tenth. Record the exact value on 3.2.4.2 spreading rate, Hc--value of H at a specified Line C of the-worksheet shown in Fig. 1. contrast ratio C. 6.6 Doctor Blade Film Applicators, width 150 mm, clear 32.4.3 hiding power, Hoss--the spreading rate at the... ances 50, 75, 100, 125, 150, 175, and 200 pm. contrast ratio C = 0.98. N' 2--With doctor blades made in the United States, estimate 25 N' 1--It should be emphasized that this contrast ratio does not represent visually complete hiding, nor does it indicate that the same mm/in. and 25 pm/mil. Bird-type applicators are usually marked with their half clearance. contrast ratio holds at every wavelength. 6.7 Computer and Software,10 for solving the relevant 4. Summary of Test Method Kubelka-Munk equations. 4.1 The reflectivity Ra of the coating is determined from 7. Procedure reflectance measurements on black and white hiding power charts: 4.2 The scattering coefficient S of the coating is deter mined from R,,, and the reflectance R0 and spreading rate Hx of a film applied on black glass. 4.3 The hiding power, H0_9i of the coating is calculated from the reflectivity and the scattering coefficient S. 4.4 As an optional procedure the contrast ratio C at a specified spreading rate Hc is calculated from and S. 7.1 General Instructions: 7.1.1 Film Application--Drawdowns should be made manually with a smooth uniform motion, at the rate of about 6 cm/s. Paper charts should be held flat by a vacuum plate or other suitable device while making drawdowns. 7.1.2 Reflectance Measurements--Measure the reflec tance of each test area at a minimum of three locations, reading or estimating to four decimal places and calculating mean values to the same. Charts should be placed over a white surface and black glass over a black surface while 5. Significance and Use measurements are being made. 5.1 This is a precise instrumental method giving results having an absolute physical significance without reference to a comparison paint. It should be used when maximum precision and minimum subjectivity are required, as in testing specification coatings or evaluating the hiding effi ciency of pigments. 5.2 Hiding power Test Method D 344 is visual instead of instrumental, and gives results that are relative to a material standard instead of absolute. It is less precise than Test Method D 2805 but more closely aligned with practical painting procedures. 7.1.3 Record Keeping--All data should be recorded on a copy of the worksheet form specified in Fig. 1. Typical data entries are shown in Fig. 2. 7.1.4 Weight Measurements--Make all weighings to 0.1 mg on the analytical balance. 7.2 Paint density, D--Determine the density in g/mL to four decimal places in accordance with Test Method D1475 and record on Line A of the worksheet (Fig. 1). Ifthe density is first determined in pounds per gallon, divide by 8.3454 to obtain it in grams per millilitre. 7.3 Nonvolatile Content, N--Sandwich 0.3 mL of paint (dispensed with a 1-mL syringe) between two previously t 6. Apparatus and Materials 6.1 Substrates: 6.1.1 Black Glass Panels,6 minimum size 200 by 200 mm, and approximately 13 mm thick. 6 Black Vitrolite and Carrara structural glasses were used originally and may still be obtainable from some local glaziers but, in general, have been replaced with black float glass. If this is not available from local glaziers it may be purchased from The Leneta Co., Box 86, Ho-Ho-Kus, NJ 07423. 7 Leneta Form 3B, available from The Leneta Co., has been found satisfactory for this purpose. An equivalent may be used. a If glass slides of this type are not readily available, use clear or translucent plastic slides instead. leneta Form P420NV, available from the Leneta Co., have been found satisfactory for this purpose. ,\ 9 A template available from Precision Gage and Tool Co., 28 Volkenand Ave., Dayton, OH 45410, has been found suitable tor this purpose. An equivalent may be used. 10 Most computers can be programmed with the relevant equations. A small pre-programmed computer is available from The Leneta Co. 382 DUP0502 97563 :e shall is. The and the ickness with a allows xm the system, s a retninous source al place 30 cm2 ilue on , dear- mate 25 ted with elevant made rate of acuum ns. reflecations, ulating over a while l on a 1 data o 0.1 nL to a 1475 density 454 to f paint viously tisfactory mslucent Co., have Hid Ave., lent may . A smalt # D2805 paint Density, D: g Nonvolatile Content, W: q Template Film Area, A: _ p Drawdowns on Charts: Drawdowns on Glass: Report (1) Hiding power Ho gB . (2) Reflectivity, ___ (3) Scattering coefficient. S _ (4) Applicator clearance___ (5) Contrast ratio, Cw_____ (6) Sample Identification Type of paint _______ Formula No_________ (7) Reftectometer description Manufacturer______ Model No.________ Geometry________ H. Alternative Hiding Power Report: Specified spreading rate, H___ Contrast ratio, C____________ ,9/mL _ (decimal traction) cm2 Chart 1 a 3 4 Mean Gw -- RolRw flo Rw w ---- FL = HR0. -- W) cw Eq Al .1 of Annex At Panel 1 2 flo M.g 3 4 Mean -- -- AND , 10W M A 1^0 93 =ns, c, /?,, where C = 0.98 H,, m2/L -- HJ S, m2/L fw m2/!- EqA1.2ofAnnexA1 EqA1.3of Annex Al . m2/U. _m2/L .pm. -Color . Batch or sample No.. .Model name . -Type --------Aperture __ -m2/L- FIG. 1 Work Sheet Form _ ft/gal .mils -ffVgal weighed slides, squeezing them together so that ther paint spreads to a diameter ofabout 45 mm. Reweigh to obtain the weight of paint sample. Separate the slides, allow the films to dry, and weigh a third time to determine the dry weight. Then calculate the nonvolatile content of the paint as a decimal fraction to four places. Run in duplicate and report the mean value to three decimal places on Line B of the worksheet (Fig. 1). 7.4 Applicator Selection--Make trial drawdowns on black and white charts at clearances of 100, 150, and 200 pm. Allow them to dry overnight and measure their contrast ratios. Based on the results select the best applicator for a contrast ratio of 0.97 0.01, which may be one of the trial applicators or one of intermediate clearance. If it seems necessary, make an additional trial drawdown to confirm the correct applicator. 7.5 Drawdowns on Glass and Charts--Using the appli cator selected from 7.4, make four drawdowns each on black glass and on black and white charts in accordance with.7.1.'l. Leave enough of the white area of each chart uncoated to permit measurement of the reflectance W. 7.6 Drying of the Films--Immediately after application place each drawdown horizontally in a well-ventilated dustfree location, with all drawdowns in close proximity to one another to assure identical drying conditions, and allow to dry a minimum of 40 h before testing. 7.7 Reflectance Measurements--On the second or third day after application measure the reflectances on all of the drawdowns within as brief a time span as possible, alter nating the measurements, between charts and glass rather than doing first all one and then the other. Enter the values of Rq , Rw, and W for charts into Section D of the worksheet, and the values of Rq for glass into Section E. 7.8 Weight of Dry Film, M--After all of the reflectances are measured, position the template on the glass panels, each in its turn, and scrape off the surplus paint with a razor blade, to leave film areas defined by the template. If the template area is not already specified, measure one of the 383. DU PO50297564 D 2805 A. Paint Density, O'______ B. Nonvolatile Content, N: _ C. Template Film Area, A- _ D. Drawdowns on Charts: E. Drawdowns on Glass: 1.246 0.499 100.2 _9/mL _ (decimal fraction) Chart 1 2 3 4 Mean Panel 1 2 3 4 Mean o 0.8755 0.8723 0.8758 0.8768 -- Rw 0.9118 0.9112 0.9117 0.9117 -- = W 0.8157 0.8158 0.8123 0.8123 -- IV) 0 0.8760 0.8785 0.8793 0.8798 -- m, g 0.4803 0.4980 0.4921 0.5082 -- H*. m2/L 12.97 12.51 12.66 12.26 -- Cw 0.9602 0.9452 0.9573 0.9473 0.9606 0.9463 0.9617 0.9449 0.9800 0.9459 Eq A1.1 of Annex At S, m2/L 98.04 97.09 99.11 96.50 90.72. Ho.gQ, m2/L 9.180 9.092 9281 9.036 9.147 w,, = = f(S, C, ft,,) where C = 0.98 Report (1) Hidha Dower H-, ,,,, 9.15 mM. 373 ft2/oal (2) Reflectivity. 0.946 (3) Scattering coefficient, S 96.7 m2/L (4) Applicator clearance 125 um 5 mils (5) Contrast ratio, C,, 0.96 (6) Sample identification Type of paint_____ Exterior Latex Gloss Color White Formula No.______ SF1436 _ Batch or sample No._ 875-1234 (7) Reflectometer description ManufacturerPhotovoltModel name Model No.670Type, Colorimeter Geometry45-deo 0-dea _ Aperture _ 20 mm H. Alternative Hiding Power Report- Specified spreading rate, H_____ 15.46 _ m2/L _ 630 _ft2/gai Contrast ratio, C_________0.949 Eq A1.2of Annex A1 Eq A1.3 of Annex A1 FIG. 2 Typical Work Sheet using i each c Hiillim Enter coin-' ajeans 8.5 desirec rate Sect1 if ,{ .. v ^ 1 * I11 * resultant films carefully to determine its- area in square centimeters to the nearest tenth. Record this value on Line C of the worksheet (Fig. 1) as the characteristic area of the template. Then scrape off each paint film carefully into a weighing dish, weight to 0.1 mg, and record the weights Min Section E of the worksheet, each value entered adjacent to the corresponding value of Rq for the same glass panel. 8. Calculation 8.1 In general, calculations should be made and recorded to four significant figures and final report values to three. Enter calculated results in the worksheet (Fig. 1). Typical entries are shown in Fig. 2. 8.2 Contrast Ration Cw and Reflectivity 2?,,--From the data entered in Section D of the worksheet calculate Cw and R,, for each of the four charts, thus: Cw= RJRw Ro, Rw,W (A1 ,, 1 '' Enter the values, as they are calculated, in the appropriate?' columns of Section D, then calculate and likewise enterthar-l . means. ' , n-ifff f 8.3 Spreading Rate Hx--From the data recorded iirthK worksheet on Lines A, B, and C and in Section E, calc the spreading rate H0 9s for each of the four glass paiS thus: AX Nx> WM where: ' Hx - spreading rate, m2/L, - A = template area, cm2, N = nonvolatile content of the paint, D = density of the paint, g/mL, and M = dry film weight, g. and enter the values in the appropriate column 8.4 Scattering Coefficient S and Hiding Power m Continuing on Section E of the worksheet (see Fig: 384 DUP0502 97565 # D 2805 using the mean value of R, from Section D, calculate for each of the glass panels, first S and then Hosa in square millimetres per litre as follows: 5 =/(i?o, Rw Hx) (A1.2) H0M = f(S, C, RJ given C - 0.98 (A1.3) gnter the values as they are calculated in the appropriate columns of Section E, then calculate and likewise enter their means. 8.5 Contrast Ratio C at a Specified Spreading Rate H--If desired, calculate the contrast ratio at a specified spreading rate using the mean values of R,, and 5 from worktable Sections D and E, of the worksheet (Fig. 1), thus: C -- f(S, H, Rf) (A1.4) 9. Report 9.1 Enter the following information on the indicated line in Fig. 1, Section G: 9.1.1 Hiding Power, Hosg--Enter the mean value of H09g from Section E, rounded to the second decimal place, onto Line G(i). If desired, multiply this value by 40.746 to obtain the value in square feet per gallon to the nearest whole number and enter it on the same line. 9.1.2 Reflectivity, R,,--Enter the mean value of Ra from Section D, rounded to three significant figures, onto Line G(2). 9.1.3 Scattering Coefficient, 5--Enter the mean value ofS from Section E, rounded to three significant figures, onto Line G(i). 9.1.4 Applicator Clearance--On Line G{4) enter the clear ance of the applicator, expressed in pm and ifdesired also in mils. 9.1.5 Contrast Ratio, Cw--Enter the mean value of Cw from Section D, rounded, to the third decimal place, onto Line G(5). 9.1.6 On Line G(6) enter the identification and brief description of the coating. 9.1.7 On Line 7(7) enter the identification and descrip tion of the reflectometer employed. 9.2 Alternative Hiding Power Report: Contrast Ratio at a Specified Spreading Rate--Enter the specified spreading rate H and the value of C calculated from 8.5, into Section H of the worksheet. This report may be in addition to or instead of conventional hiding power H09g. 10. Precision 10.1 Precision--The precision values given for this test method are based on two series of interlaboratory tests. For gray and chromatic paints (6), five operators in five labora tories tested four gloss enamels covering a broad range of colors. For white paints (5), five operators in five laboratories tested three white finishes covering the range of gloss to flat. The between-Iaboratory coefficients of variation were found to be those shown in Table 1. 11. Index Terms 11.1 This test method is indexed under the following terms: hiding power (of paints/coatings); spreading rate; contrast ratio; scattering coefficient. TABLE 1 Precision of Hiding Power, HaM Maximum Acceptable Differences Coefficient of for Two Results Variation Repeatability Reproducibility Gray, and chromatic gloss finishes, % White finishes: Gloss, % Semigloss and fiat. % 3.5 1.2 5.0 <10.4 <4.7 <16.3 10.4 4.7 16.3 opriate er their in the :alculate panels. ction E. 385 DUPO 50297566 D 2805 ANNEX (Mandatory Information) ANNEX Al. KUBELKA-MUNK EQUATIONS USED IN THIS TEST METHOD itn +W-R,,,\ (AI.l) (Al.1.1) (Ai.1.2) `3 fe-*-) /T =r[/la +. li6-0cc\j* " ir2. i -c 1.60 C' S=f(R0,R,,,Hx) ." b=m~) = \.{-k-R~) s =EzxMzMz\ 2b ,n \l - Ho/lJ. (A 1.2) (Al.2.1) (Al.2.2) H -- S/P C=f(S,H,RJ P = S/H '"Jru,->-3 (**-) Hc=f(S,C,RJ --^>-5(ib*-) (A1.3) (A1.3.I) C = . a.+ b coth bP - 0.80 (a +i b coth bP) [1 - 0.80(a - b coth bP)] (A1.3.4L (A 1.3.5) (A 1.4) (A 1.4.1) (Al.4.2); (A 1.4.% ' (Al.4.4) | | REFERENCES Ji (X) Kubelka, P., and Munk, F., "Ein Beitrage zur Optik der Farbenstriche," Zeitzchriftfur Technische Physik, Vol 12, 1931, p. 593. (2) Steele, F. A., "The Optical Characteristics of Paper," Paper Trade Journal, Vol 100, No. 12, 1935, p. 37. (3) Kubelka, Paul, "New Contributions to the Optics of Light Scat tering Materials," Journal of the Optical Society ofAmerica, Vol 38, 1948, p. 448. (4) Switzer, M. H., "Equations for Calculating Contrast Hiding Index and Spreading Rate of Paints," ASTM Bulletin No. 181, 1952, P- 75. (5) Jacobsen,- A. E., Mitton, P. B., and Switzer, M. H., "Determination ofthe Hiding Power of Nonchromatic Paints," Materials Research and Standards, Vol 2, No. 12, 1962, pp. 1004-1005. (6) Mitton, P. B., Madi, A. J., and Rode, J., "Development of a Test Method for Hiding Power," Journal ofPaint Technology, Vol 39, No. 512, 1967, pp. 536-543. (7) Mitton, P. B,, "Easy Quantitative Hiding Power Measurements,' Journal ofPaint Technology, Vol 42, No. 542, 1970, pp. 159-183. 11 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if notrevised, either reapproved or withdrawn. Your comments are invitedeither for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. %\ 3S<? DUPO 50297 567 (Al.3.3) (Al.3.4) (Al.3.5) (A 1.4) (A 1.4,1) (A 1.4.2) (Al.4.3) (A 1.4.4) termination its Research nt of a Test igy, Vol 39, surements," p. 159-183. I Designation: D 2830 - 91 Standard Test Method for Durability and Compatibility of Factory-Primed Wood Products with Representative Finish Coats1 This standard is issued under the fixed designation 2830; the number immediately following the designation indicates the. year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method provides for the determination ofthe relative durability and compatibility of factory-primed wood and wood-based substrates with representative finish coats when exposed to the weather. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user ofthis standard to establish appro priate safety and health practices and determine the applicar-bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D659 Method of Evaluating Degree of Chalking of Exterior Paints2 D660 Test Method for Evaluating Degree of Checking of Exterior Paints2 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints2 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints2 D714 Test Method for Evaluating Degree of Blistering of Paints2 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints2 D1006 Practice for Conducting Exterior Exposure Tests of Paints on Wood2 D3274 Test Method of Evaluating Degree of Surface Disfigurement of Paint Films by Microbial (Fungal or Algal) Growth or Soil and Dirt Accumulation2 D3359 Test Methods for Measuring Adhesion by Tape Test2 2.2 U. S. Federal Standards? TT-P-96b TT-P-102 3. Summary of Test Method 3.1 This test method consists ofthe atmospheric exposure of at least three types of conventional exterior white house paints applied to panels of factory-primed wood or woodbase substrates that have been exposed to atmospheric ' This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.52 on Factory-Coated Wood Building Products. Current edition approved Oct. 15, 1991. Published December 1991. Originally published as D 2830 - 69. Last previous edition D 2830 - 82 (1987). 2 Annual Book ofASTM Standards, Vol 06.01. 3 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn! NPODS. weathering conditions for periods of 0, 3, and 6 months. 3.2 The finish coats are applied by brush. 3.3 An additional panel of original factory-primed sub strate, without finish coat, is exposed for the duration of the test. 4. Significance and Use 4.1 This test method is useful for evaluating the weath ering performance of factory-applied primers on wood or wood-based substrates overcoated with a field-applied top coat. 4.2 This test method is useful for evaluating the weath ering compatibility of commercial topcoats over factoryapplied primers on wood or wood-based substrates. 5. Apparatus 5.1 A vertical (90 from horizontal) test fence constructed in accordance with requirements of Practice D 1006. 6. Materials 6.1 Exterior Finishes: 6.1.1 Paint, Oil, Alkyd, fume resistant, conforming to Federal Specification TT-P-102. 6.1.2 Resin Latex Paint, Synthetic, of the emulsion type designed for use on exterior wood surfaces (such as TTP-96b). 6.1.3 Flat Alkyd, Solvent-Thinned, Exterior. 6.1.4 Any other type of exterior finish paint mutually agreed upon. 6.2 Bristle Brush (Natural or Synthetic). 7. Procedure 7.1 The minimum length of panel is 3 ft (910 mm) with a minimum width of 6 in. (150 mm) of a particular preprimed substrate. 7.2 Mark off one third of the panel area (in a manner which will not damage the prime coat) and apply by brush to the right one third panel area a single coat ofone ofthe white finishes at a spreading rate as recommended by the manufac turer or by the appropriate Federal specification. Paint the panel and dry indoors for 7 days under prevailing conditions of temperature and humidity, taking care to avoid exposure to drafts or excessive heat. 7.3 Determine the spreading rate of the finish paints by the weight difference method or other suitable methods. Record the spreading rate, film thickness, and method used. 7.4 Fasten the panel to a south exposure rack. No t e 1--Panel mounting should be the same as normal practice for the mounting of a particular substrate. 387 DU PO 502 97568 # D2830 7.5 After 3 months (1 week) of exposure of the panel, coat the center one third section adjacent to the section already coated with exterior finish as specified in 7.2. No t e 2--If possible, the application should be made in the labora tory as in 6.2. No washing or cleaning should be done to the surface to be coated. 7.6 At completion of 6 months (1 week) of exposure to the weather, apply finish coat to the final third section of the panel as specified in 7.2. 7.7 Examine each section of the panels visually for appearance, mildew, and film failure at intervals of not more than 3 months (preferably 1 month) beginning 1 month after initial exposure. 7.8 At the end of each 6 months exposure of a topcoated section, test for intercoat adhesion between the factoryapplied primer and the topcoat as follows: 7.8.1 Cut a small "X" in the film with a sharp knife or razor blade. The cuts should penetrate the substrate slightly but not distort the film unduly. Apply pressure-sensitive tape4 so that it crosses the "X" in the direction of the acute angles. Press the tape on carefully with the flat surface of the- ____________ 4 3-M Company's No. 600 Cellophane Tape has been found satisfactory. Tape shall be stored in an airtight container and shall not be more than 6 months old. fingernail or with a rubber eraser. Remove the tape with a quick yank, at a 90 angle to the surface. 7.9 Exposure of the topcoated preprimed substrate may be terminated 12 months after application of the finish coat to the third section. Additional exposure may be agreed upon between buyer and seller. 8. Report 8.1 Report the following properties: 8.1.1 Chalking--Method D 659. 8.1.2 Checking--Test Method D 660. 8.1.3 Cracking--Test Method D 661. 8.1.4 Erosion--Test Method D 662. 8.1.5 Flaking--Test Method D 772. 8.1.6 Blistering--Test Method D 714. 8.1:7 Intercoat Adhesion--Test Methods D 3359. 8.1.8 Mildew--Test Method D 3274. 9. Precision and Bias f 9.1 Varying weather conditions from year to year and at I several exposure sites predude development of predsion and t bias data. ! 10. Keywords , : | l^.l adhesion; factory primed wood; primer performance; j f topcoat Compatibility; weathering J? The American Society lor Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination Of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Commktao an Standards, 191S Race St., Philadelphia, PA 19103. 5i- pro noi f frac l Aert Are! pt Aspl Aspl Bitu Blea Coil Elec Hou Indi Lact Late Late Mag Plas Pow She Sob Tra Var 388? DU P0502 97569 tape with a bstrate may a finish coat agreed upon 59. year and at ecision and aformance; Designation: D 2832 - 83 (Reapproved 1991)f1 Standard Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings1 This standard is issued under the fixed designation D 2832; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year ofJast revision. A number in parentheses indicates the year of last reapproval, A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. N' --Keywords were added editorially in June 1991. j. Scope 1.1 This guide is intended to aid in the selection of the proper ASTM standard for determining the volatile and nonvolatile content of paint and related coatings. No t e--Test methods for determining the composition of the volatile fraction are not covered by this guide. j. 1.2 The standards included are as follows: Type of Coating Section ASTM' Designation Aerosol coatings Architectural wall coatings, interior, high performance Asphalt roof coatings Asphalt roof coatings, aluminum-pigmented Bitumens, emulsified Bleached lac varnish Coil coatings Electrical insulation varnishes House paints, gloss Industrial baking enamel Lacquers, clear and pigmented Latex paint, exterior Latex paint, interior Magnet wire enamels Plastics, coatings for Powder coatings Shellac varnish, orange Solvent-reducible coatings Traffic paints Varnishes Wall and trim enamels, interior semigloss, solvent-based Wall paints, flat Water-reducible coatings 4.1 D 3062 4.3 , D 1644 4.4 D2823 4.5 D2824 4.6 D2939 4.7 D 1650 4.8 D 1353 D2697 4.9 D 115 4.10 D2697 4.10 D 2697 4.11 D 1644 D333 4.10 D2697 4.10 D2697 4.12 D 3288 4.13 D 1644 4.14 D 3451 4.7 D1650 4.2 D 2369 4.15 D2205 4.16 D 1644 4.17 D2697 4.10 D2697 4.2 D 2369 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: > This guide is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paint and Paint Materials. Current edition approved March 9, 1983. Published September 1983. Origi nally published as D 2832 -69. Last previous edition D 2832-69 (1980). D115 Methods of Testing Varnishes Used for Electrical Insulation2 D333 Test Methods for Clear and Pigmented Lacquers3 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Re lated Products4 D1644 Test Methods for Nonvolatile Content of Varnishes3 D1650 Methods of Sampling and Testing Shellac Varnish5 D 2205 Guide for Selection of Tests for Traffic Paints3 D2369 Test Method for Volatile Content of Coatings3 D2697 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings3 D 2823 Specification for Asphalt Roof Coatings6 D2824 Specification for Aluminum-Pigmented Asphalt Roof Coatings6 D 2939 Method of Testing Emulsified Bitumens Used as Protective Coatings6 D3062 Test Method for Solids Content of Aerosol Coatings7 D 3288 Method of Testing Magnet-Wire Enamels8 D3451 Practices for Testing Polymeric Powders and Powder Coatings3 3. Significance and Use 3.1 The nonvolatile content of paint and related coatings is useful to producers and users and to environmental and health and safety interests in comparing the coverage of competing products and in estimating the volatile organic content. 4. Procedure 4.1 Aerosol Coatings--Test Method D3062 covers the determination of solids content (weight %) in aerosol coat ings. 4.2 Volatile Content ofCoatings ( Test Method D 2369)-- This test method covers the determination of the volatile content of coatings. It is considered to be applicable to most 2 Annual Book ofASTM Standards. Vol L0.01. 3 Annua! Book ofASTM Standards, Vol 06.01. * Annua! Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vol 06.02. 6 Annual Book ofASTM Standards, Vol 04.04. 7 Annual Book ofASTM Standards, Vol 15.09; 8 Annual Book ofASTM Standards. Vol 10.02. 389 DU P050297570 m D 2832 solvent-reducible and water-reducible paints. 4.3 High Performance Interior Architectural Wall Coat ings (HIPAC)--Determine the nonvolatile content of HIPAC coatings in accordance with Test Methods D 1644. Calculate the volatile content (weight %) by difference. 4.3.1 Method A--3 h at KWC for paints with nonsolvent components that decompose at higher temperature. 4.3.2 Method B--10 min at 149C for most paints with nonsolvent components that are reasonably stable at 149C. 4.4. Asphalt Roof Coatings--Determine the nonvolatile content (weight %) of asphalt roof coatings of brushing or spraying consistency in accordance with 8.2 of Specification D 2823. 4.5 Aluminum-Pigmented Asphalt Roof Coatings--The nonvolatile content (weight %) of asphalt-based aluminum roof coatings suitable for application to roofing or masonry surfaces by brush or spray is determined in.accordance with 8.2 of Specification D 2824. 4.6 Emulsified Bitumens Used as Protective Coatings-- Section 8 of Test Methods D 2939 contains a method for determining residue by evaporation (weight %) of emulsified bitumens used in relatively thick films as protective coatings for metals and built-up roofs. 4.7 Shellac Varnish.--Determine the nonvolatile matter in orange shellac and bleached lac varnishes in accordance with Sections 14 through 16 of Methods D 1650. 4.8 Coil Coatings--Although stated to be for solvents, determine the nonvolatile matter (weight %) in accordance with Test Method D 1353. Determine volume solids in accordance with Test Method D 2697. 4.9 Electrical Insulation Varnishes: 4.9.1 Sections 18 through 22 of Methods D115 on nonvolatile matter by weight, are applicable to the following classifications of varnishes used for electrical insulation: alcohol-soluble varnishes, oxidizing air-drying varnishes, thermosetting varnishes, oxidizing baking varnishes, air drying asphaltic varnishes, silicone varnishes, and thermo setting laminating varnishes. 4.9.2 Determine nonvolatile matter in electrical insulating varnishes intended for electrical equipment operating at 180C and above in accordance with Methods D 115 except that the temperature used shall be 275 5.5T (135 3C) or at a temperature agreed upon between the producer and the user. 4.10 Volume Nonvolatile Matter in Clear or Pigmented Coatings (Test Method D 2697)--This test method is appli cable to the determination of the volume nonvolatile matter of coatings. A gloss enamel, a flat wall paint, a gloss house paint, an industrial baking enamel, an interior latex paint, and an exterior latex paint included in formal collaborative studies of this test method. 4.11 Lacquer Coatings--Determine the nonvolatile con. tent of clear and pigmented lacquers as described in Test Methods D1644. As an additional requirement, the spec, imen shall be reheated and reweighed until the weight is constant to within 1 mg. Method A of Test Methods D 1644 is preferred since Method B is potentially dangerous when used with lacquers. 4.12 Magnet Wire Enamels--Sections 17 through 23 of Test Method D 3288 cover the determination of nonvolatile content (weight %) in magnet wire enamels. 4.13 Coatingsfor Plastics--Determine nonvolatile matter in clear and pipiented coatings designed for use on rigid or semirigid plastic substrates in accordance with Test Methods D 1644. 4.14 Polymeric Powders and Powder Coatings--Deter- mine nonvolatile content (weight %) in accordance with Section 12 of Practices D 3451. Determine volatile content at baking or fusion temperature in accordance with Section 13 of Practices D 3451. 4.15 Traffic Paints--Determine the nonvolatile content of traffic paints, ready-mixed, of spraying consistency of the premix, drop-in, or combination type in accordance with Test Methods D 1644, and state any necessary larger spec imen size for beaded paint Either of the two methods can be used as follows: 4.15.1 Method A--3 h at 105C for paints with nonsolvent components that decompose at higher tempera ture. 1 4.15.2 Method B--10 min at 149C for most paints with nonsolvent components that are reasonably stable at 149T, 4.16 Varnishes--Nonvolatile content (weight %) of var nishes is determined using Test Methods D 1644. These test methods may give high results due either to incomplete elimination of volatile matter or to absorption of oxygen by oxidizing-type varnishes. 4.17 Solvent-Based Interior Semigloss Wall and Trim, Enamels--Use Test Method D 2369 to determine volatile content. Volume nonvolatile matter is determined in accor dance with Test Method D 2697. 5. Precision 5.1 Some of the referenced ASTM standards have preci sion limits. Reference to the individual standards for preci sion statements is recommended. 6. Keywords 6.1 nonvolatile content of paints and related coatings; volatile content of paints and related coatings I 1T Relate D01.4 Cur publis! The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ol Infringement ofsuch rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, eitherreapproved or withdrawn. Yourcomments are invitedeither forrevision oltNs standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. | 390 DUP050297571 borative tile conin Test he specveight is ; D 1644 us when jh 23 of i volatile e matter rigid or Methods --Deterice with content Section content y of the ice with ,er specs can be ts with empera- nts with t 149C. of vartese test omplete ygen by d Trim volatile a accor- Designation: D 2833 - 89 Standard Index of Methods for Testing Architectural Paints and Coatings1 This standard is issued under the fixed designation D 2833; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reappraval. Scope 1.1 This index is provided for reference in the selection of procedures, test methods, and specifications to be used in the evaluation of architectural paints and coatings designed for application in the field. Composition specifications and analytical methods in general, also tests on raw materials, are pot included, the scope being limited to procedures required in the evaluation of finished coatings. 1.2 Methods suitable for both interior and exterior coat ings of either the water-thinned or solvent-thinned type are listed by ASTM designation primarily. Where comparable (hut not necessarily identical) methods exist in U.S. Federal jest Method Standard No. 141, the Federal Method num bers are also listed. 1.3 Where more then one test method is listed for the same characteristic in this index, no attempt is made to indicate superiority of one test method over another. Selec tion of the test methods to be followed must be governed by experience and the requirements in each individual case, 1 This index is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee CO] ,42 on Architectural Finishes. Current edition approved March 31, 1989. Published May 1989. Originally published as D 2833 - 69. Last previous edition D 2833 - 83. together with agreement between the purchaser and the seller. 2. Precision and Bias 2.1 If available, precision for any procedure or test method selected is given in the latest issue of the subject standard. 3. Test Categories 3.1 For- convenience in selection, the procedures, methods, and specifications listed in this index are classified into three groups and three classes. The category of each listing is indicated in a column preceding the reference. The classifications are as follows: 3.1.1 Group I--Applicable to Either Water- or SolventReducible Coatings: Class A--For both interior and exterior products. Class B--For interior products only. Class C--For exterior products only. 3.1.2 Group II--Water-Thinned Coatings: Class A--For both interior and exterior products. Class B--For interior products only. Class C--For exterior products only. 3.1.3 Group III--Solvent-Thinned Coatings: Class A--For both interior and exterior products. Class B--For interior products only. Class C--For exterior products only. : precir preci- oatings; 391 DUP0502 97572 # D 2833 INDEX OF METHODS Category JA Definitions of Terms Relating to Paints, Varnishes, Lacquers and Related Products. Examination of Paint Products IA Prtmers and Primer Surfacers over Preformed Metal IA Sampling Liquid Paints and Related Pigmented Coatings IB Testing High-Performance Interior Architectural Wall Coatings IIA Resistance of Emulsion Paints in the Container to Attack by Microorganisms HA Water-Borne Floor Paints IIB Latex Flat Wall Paints JIB interior Latex Semigloss and Gloss Paints IIC Testing Asphalt Emulsions for Use as Protective Coatings for Metal IIC Exterior Latex House Paints IIIA Testing Varnishes IIIA Clear and Pigmented Lacquers IIIA Solvent-Reducible Floor Paints IIIB Performance Tests of Clear Poor Sealers 1118 Sampling and Testing Shellac Varnish IIIB Interior Solvent-Reducible Flat Wall Paints IIIB Solvent-Reducible Interior Semiglosd Wall arid Trim Enamels me Exterior Solvent-Reducible House and Trim Paints ,:r ASTM Volume No, 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 A 06.01 06.01 06.01 06.01 06.01 06.02 06.01 06.01 06.01 Physical Tests IA Density of Paint, Varnish, Lacquer and Related Products IA Evaluating the Degree of Settling of Traffic Paint IA Flash Point of Liquids by Setaflash Closed-Cup Apparatus IA Flash Point by Pensky-Martens Closed Tester IA Coarse Particles in Pigments, Pastes, and Paints IA Fineness of Dispersion of Pigment-Vehicle Systems IIA Package Stability of Latex Paint IIA Freeze-Thaw Resistance of Water-Borne Paints IIA Freeze-Thaw Stability of Multicolor Lacquers IIA Particle Size of Multicolor Lacquers IIIA Flash Point by Tag Closed Tester IIIA Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus IIIA Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25"C IIIA Color of Transparent Liquids (Gardner Color Scale) 06.01 06.01 06.03 06.03 06.01 06.01 06.01 06.01 06.01 06.01 06.03 06.03 06.03 06.01 , Rheological Properties IA Consistency of Paints Using the Stormer Viscometer IA Leveling of Paints by Draw-Down Method IA Viscosity by Ford Viscosity Cup IA Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield) Viscometer IA High Shear Viscosity Using ICI Cone/Plate Viscometer IA Sag Resistance Using a Multinotch Applicator IIIA Viscosity of Transparent Liquids by Bubble Time Method IIIA Flow Ratings of Organic Coatings Using the Shell Flow Comparator Panel Specifications and Preparation IA Preparation of Zinc-Coated Galvanized Steel Surfaces for Painting IA Preparation of Hot-Dipped Nonpassivated Galvanized Steel for Testing Paint IA Pictorial Surface Preparation Standards for Painting Steel Surfaces IA Preparation of Steel Panels for Testing Paint, Varnish, LacquBr, and Related Products 1C Wood to Be Used in Panels in Weathering Tests of Coatings 1C Making and Preparing Concrete and Masonry Panels for Testing Paint Finishes IIIA Preparation of Aluminum and Aluminum-Alloy Surfaces for Painting IIIA Preparation of Hot Dip Aluminum Surfaces for Painting Film Preparation and Thickness IA Producing Films of Uniform Thickness of Paint, Varnish, Lacquer, and Related Products on Test Panels IA Measurement of Wet Film Thickness of Organic Coatings IA Measurement of Dry Film Thickness of Organic Coatings Using Micrometers IA Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base IA Nondestructive Measurement of Dry Film Thickness on Nonconductlve Coatings Applied to a Nonferrous Metal Base IA Microscopic Measurement of Dry Film Thickness of Coatings on Wood Products * Discontinued; see 1980 Annual Book of ASTM Standards, Part 27. 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 ASTM Designation D16 D3322 D3925 D3730 D2574 D3366 D2931 D 4S40 D1010 D3129 D154 D333 D3383 D1546 D1650 D3323 D3425 D2932 D1475 D869 D3278 093 D185 D1210 D1849 D2243 D2337 D2338 D 56 D1310 D1963 D1544 662 D40S2 1200 D 2196 D 4287 D 4400 D1545 D2353 D2092 D2201 D2200 D 609 0 358 D1734 D1730 D1731 D823 D1212 D1005 D1186 D1400 D 2691 392 Federal Standard No. 141 1022,3011 2011.1 Category IA IIIA IA IA IA IA IA IA IA IA IA IA IA IA IA IB IA IA IA IA IIIA IIIA IIIA IIIA IIIA IIIA IIIA IIIA IIIA IA IA IA IA IA IA IA IA IA IB IB IB 1C 1C 1C 1C 1C 1C DUP050297573 # D2833 INDEX OF METHODS--Conf/m/ed Category ASTM - Volume No. Drying and Curing IA Drying, Curing or Film Formation of Organic Coatings at Room Temperature illA Gas Checking and Draft Tests of Varnish Films Porosity and Permeability 06.01 06.01 !A Water Vapor Permeability of Organic Coatings Rims IA Porosity of Paint Rims 06.01 06.01 Appearance Properties Gloss, Reflectance, and Hiding Power IA Specular Gloss IA 45-deg 0-deg Directional Reflectance of Opaque Specimens by Rlter Refledometry 06.01 06.01 IA Hiding Power of Paints by Reflectometry 06.01 IA Relative Dry Hiding Power of Painis by Visual Evaluation of Brushouts 06.01 IA Computing the Color of Objects Using the CIE System IA Specifying Color by the Munsell System iA Visual Evaluation of Color Differences of Opaque Materials IA Calculation of Color Differences from Instrumentally Measured Color Coordinates 14.02 06.01 06.01 06.01 IA Selecting and Defining Color and Gloss Tolerances of Opaque Materials and for Evaluating 06.01 Conformance IA Paint Spatter Resistance to Roller Application IA Reflective Haze of High Gloss Surfaces IB Uniformity of Appearance *' 06.01 06.01 06.01 Physical Strengths and Resistance (Nonchemical) IA Preparation of Uniform Free Rims of Organic Coatings IA Tensile Properties of Organic Coatings IA Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact) IA Measuring Adhesion by Tape Test IllA Mandrel Bend Test of Attached Organic Coatings IllA Elongation of Attached Organic Coatings with Cylindrical Mandrel Apparatus IllA Elasticity or Toughness of Varnishes IllA Print Resistance of Lacquers IllA Abrasion Resistance of Organic Coatings by Air Blast Abrasive IllA Abrasion Resistance of Organic Coatings by Falling Abrasive IllA Abrasion Resistance of Clear Floor Coatings IllA Indentation Hardness of Organic Coatings IllA Adhesion of Organic Coatings by Scrape Adhesion 06.01 06.01 06.01 06.01 06.01 B 06.01 06.01 06.01 0S6.01 06.01 06.01 Resistance to Chemicals and Environment IA Color Permanence of White Architectural Enamels 06.01 IA Effect of Household Chemicals on Clear and Pigmented Organic Finishes 06.01 IA Fire Retardancy of Paints (Cabinet Method) 06.01 IA Fire Retardancy of Paints (Stick and Wick Method) C IA Finishes on Primed Metallic Substrates for Humidity-Thermal Cycle Cracking 06.01 IA Water Resistance of Coatings in 100 % Relative Humidity 06.01 IA Coatings Designed to Be Resistant to Elevated Temperatures During Their Service Life 06.01 IA Surface Burning Characteristics of Building Materials IA Surface Flammability of Materials Using a Radiant Heat Energy Source 04.07 04.07 IB Resistance to Growth of Mold on the Surface of Interior Coatings in an Environmental 06.01 Chamber IB Washability Properties of Interior Architectural Coatings 08.01 IB Humid-Dry Cycling for Coatings on Wood and Wood Products 06.01 1C Operating Light- and Water-Exposure Apparatus (Carbon-Arc Type) for Testing Paint and 06.01 Related Coatings and Materials IC Accelerated Testing of Moisture Blister Resistance of Exterior House Paint on Wood B 1C Corrosion Resistance of Coated Steel Specimens (cycEc method) 06.01 IC Evaluating Degree of Surface Disfigurement on Paint Films by Microbial (Fungal or Algal) 06.01 Growth or Soil and Dirt Accumulation IC Determining by Exterior Exposure the Susceptibility of Paint Films to MicrobiologicalAttack 06.01 IC Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Rame Carbon-Arc Type) 08.01 for Testing Paint, Varnish, Lacquer, and Related Products Using Dew Cycle IIA Stain Removal from Multicolor Lacquers 06.01 IIB Scrub Resistance of Interior Latex Flat Wall Paint 06.01 118 Efflorescence of Interior Latex Paints 06.01 IllA Testing Water Resistance of Coatings Using Water Immersion 06.01 IllA Light Stability of Clear Coatings 06.01 IllA Testing Water Resistance of Coatings Using Water Fog Apparatus 06.01 B Oisoontlnued; sea 1988 Annual Book ofASTM Standards, Vol 06.01. Discontinued; see 1976 Annual Book of ASTMStandards, Part 27. 393 ASTM Designation 01640 D1643 D1653 D 3258 0 523 E 97 D 2805 D 344 E 308 D 1535 D 1729 D 2244 D3134 D 4707 D 4039 D 3928 D4708 D 2370 D2794 D 3359 D 522 D 1737 D 1642 D 2091 D 658 D 968 D1395 D 1474 D2197 D 1543 D 1306 D 1360 D1361 D 2246 D 2247 D 2485 E 84 E 162 D 3273 D3450 D3459 D822 D 2366 D 2933 D 3274 D3456 D3361 2198 D 2486 D1736 D 870 D2620 D1735 Federal Standard No. 141 4061.1 6221 D UP050297574 # 0 2833 INDEX OF METHODS--Continued Category ASTM Volume No. Resistance to Chemicals and Environment IIIA Salt Spray (Fog) Testing 06.01 IIIA Acetic Acid-Salt Spray (Fog) Testing IIIA Temperature-Change Resistance of Clear Nitrocellulose Lacquer Films Applied to Wood 06.01 m Resistance of Dried Films of Varnishes to Water and Alkali 06.01 IIIA Detergent Resistance of Organic Coatings 06.01 me Evaluation of Painted or Coated Specimens Subjected to Corrosive Environment 06.01 Durability Tests IA Evaluating Degree of Blistering of Faints 06.01 IA Water Resistance of Coatings Using Controlled Condensation 06.01 1C Conducting Tests on Paints Using Fluorescent UV-Condensation Light- and Water- 06.01 . Exposure Apparatus 1C Durability and Compatibility of Factory-Primed Wood Products with Representative Finish 06.01 Coats 1C Evaluating Degree of Chalking of Exterior Paints 06.01 1C Evaluating Degree of Cheeking of Exterior Paints 06.01 . 1C Evaluating Degree of Cracking of Exterior Paints 06.01 1C Evaluating Degree of Erosion of Exterior Paints 06.01 1C Evaluating Degree of Flaking (Scaling) of Exterior Paints 06.01 , 1C Conducting Exterior Tests of Paints on Wood 06.01 1C Single- and Multipanel Forms for Recording Results of Exposure Tests of Paints 06.01 lie Reporting Paint Film Failures Characteristic of Exterior Latex Paints 06.01 IA Evaluating Degree of Rusting on Painted Steel Surfaces 06.01 me Conducting Exterior Exposure Tests of Paints on Steel 06.01 me Exterior Durability of Varnishes 06.0T ASTM Designation B 117 B 287 D 1211 D 1647 D 2248 D1654 D 714 D 4585 D 4587 D 2830 D 669 D660 . D 661 D 662 D 772 1006 D1150 D 1048 D 610 D1014 D 1641 Federal Standard No. 141 The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee^ and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of thisstandard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you feel that your comments have not received a fear hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 3. Si 3.1 come lent-t This) signif 394 DU PO 502 97575 il Standard x 141 Designation: D 2921 - 88 Standard Test Method for Qualitative Tests for the Presence of Water Repellents and Preservatives in Wood Products1*2 This standard is issued under the fixed designation D 2921; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A numberin parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope L.l This test method describes simple qualitative field or laboratory tests to determine water repellency or the pres age of chlorinated phenol3 preservative chemicals in wood products that are specified to be water repellent preservative treated. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its, use, It. is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2, Referenced Documents 2.1 U.S. Federal Specification: TT-W-572 Wood Preservative Water-Repellant4 2.2 NIST Standard: 262-63 Water Repellent Preservative Non-Pressure Treat ment for Mill Work5 3, Significance and Use 3.1 Although chlorinated phenol-treated wood has be come less common due to environmental concerns, repel lent-treated wood is commonly specified in construction. This test method provides a means to verify the presence ofa significant level of water repellent protection. 4. Apparatus 4.1 Eyedropper, plastic squeeze bottle or similar means for metering drops of water. 4.2 Flame Source, such ais bunsen burner, butane torch, or alcohol burner. 4.3 Copper Wire Coil Specimen Holder {or Other Suitable Copper Holder)--A suitable copper wire coil can be made by using a lead pencil as a mandrel to form a helix using copper wire of about `As to V32 in. (1.6 to 2.4 mm) in diameter. Leave a space of approximately the diameter of the wire between each loop. The helix should be % to 1 in. (19 to 25 mm) in length. Leave a pigtail of about 6 in. (152 mm) of wire at one end of the helix and form a loop of approxi 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint tsd Related Coatings and Materials and is the direct responsibility of Subcom mittee DOt,52 on Factory-Coated Wood Products. ] Current edition approved March 25, 1988. Published May 1988. Originally Published as D 2921 - 70. Last previous edition D 2921 - 70 (1979){|. 2 An improved quantitative test method for water repellenls is under develop ment by Subcommittee DO 1.42. ! Pentachlorophenol, tetrachiorophenol and other chlorinated phenols. * Available from Standardization Documents Order Desk, Bldg. 4 Section D, \ IPO Robbins Ave., Philadelphia, PA 19111-5094, Attn; NFODS. _1 Available from the National Institute of Standards and Technology, MD 20899. mately. 1 in. (25 mm) in diameter to be used as a holder for the coil. 4.4 Sharp Knife. - 5. Water Repellent Test 5.1 Place uncut wood items to be tested so that the end grain is exposed as a horizontal surface. If the end grain cannot be so positioned, comparisons can be made on the flat grain. 5.2 With an eye dropper, or similar device, allow several drops of water to fall from about lh in. (13 mm) on the end grain of the wood. Wait 5 min and then observe the degree of penetration. With flat grain or vertical grain surfaces, waiting periods of 10 to 15 min may be necessary. 5.3 Water drops that immediately flatten out, penetrate and darken the wood, indicate that the wood has not been treated with a water repellent. 5.4 Water drops that "bead-up" and remain as spheres, with little or no color change or penetration, indicate that the wood has been treated with a water repellent. Water repellent preservatives, meeting Fed. Spec. TT-W-572 and NBS Stan dard 262-63, impart sufficient water repellency to the end grain of wood to cause water drops to bead up and form spheres. 6. Preservative Test 6.1 Chlorinated phenol based wood preservatives emit a characteristic green flame upon pyrolysis within a ventilated copper envelope due to the release of chlorine and its consequent reaction with copper (Beilstein's test). Untreated wood produces a yellow-orange flame but any chlorine containing compound will give a positive test. 6.2 Using the copper wire specimen holder, described in 3.3, hold the coil portion id the flame until it bums with a characteristic yellow-orange color. This preheated coil is then allowed to cool. 6.3 With a knife, cleaned by heating after each use, cut a splinter from the specimen of wood to be tested. Samples should be taken near the end of the wood items where end grain is exposed and where normal concentration of the preservative chemicals is greatest. The size of the wood sample should be smaller than the length and inner diameter of the coil. 6.4 With the copper coil held horizontally, place the splinter in the center of the coil. Put the copper coil with wood splinter in the flame and bum. If chlorinated phenols are present, the characteristic green flame is produced. Untreated wood produces the yellow-orange flame. 7. Accuracy 7.1 The tests are less accurate on flat grain and the 395 DU PO 502 97576 # D2921 heartwood of some wood species, so that ehd grain and sapwood should be used whenever possible. 7.2 Tests on both a known untreated sample and a treated sample of the same wood species will provide comparison standards for the operator and will improve the accuracy of the tests. 7.3 Test results are improved if tests are made with wood samples taken from the center ofa stack or from a protected area where the possibility of contamination is least Untreated items which come in physical contact with pre servative treated products during handling and shipping m- show slight evidence of the preservative chemical. ^ 7.4 More than one wood sample obtained from differem areas from the unknown piece should be tested. 8. Precision and Bias 8.1 No numerical statement ofprecision is possible in % qualitative test method. One hundred percent agreement ^ obtained in a round-robin test. 8.2 Bias--Bias has not been determined. [ j The American Society tor Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any item mentioned In this standard. Users of this standard ere expressly advised Mat determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any lime by the responsible technical committee and must be reviewed every five years and H not revised, either reepproved or withdrawn. Your comments areInvited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Race St., Philadelphia, PA 19103. 1. Scope 1.1 Tb f0r testin methods 1.2 Tl applicath paeans,, previous) surfaces. 1.3 Ti ations, c address < the resp appropri applicab 2. Refer 2.1 A D16 and D 185 Pas D 34^ the D52: Or D52 D56 St< D82 Tl Te D 12 me D 14 qu D 15 an 396 DUPO 502 97577 Designation: D 2931 - 84 {Reapproved 1989)e1 n different ;ible in this ement was Standard Guide for Testing Latex Flat Wall Paints1 This standard is issued under the fixed designation D 2931; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. ei N' --The title was editorially changed in March 1989. j. Scope 1.1 This guide covers the selection and use of procedures for testing flat latex paints for use on interior walls. The test methods included are listed in Tables 1 and 2. 1.2 This guide applies to ready-mixed flat latex paints for application by brushing, roller coating, spraying, or other means, on plaster, masonry surfaces, wood, wallboard, previously painted surfaces and other interior architectural surfaces. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. t Referenced Documents 2.1 ASTM Standards: D 16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts4 D 522 Test Method for Mandrel Bend Test of Attached Organic Coatings4 D 523 Test Method for Specular Gloss4 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer4 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels4 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems4 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products4 D1554 Definitions of Terms Relating to Wood-Base Fiber and Particle Panel. Materials5 ' These practices are under the jurisdiction of ASTM Committee D-l on Paint, tad Related Coatings and Materials and are the direct responsibility of Subcom mittee DO 1.42 on Architectural Finishes. Current edition approved Aug. 31, 1984. Published January 1985. Originally Published as D 293! - 70 T. Last previous edition D 2931 -79. 2 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 2 Annual Book ofASTM Standards.Vols 06.0T and 06.02. ............... * Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vol 04.09. D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature4 D1729 Practice for Visual Evaluation ofColor Differences ofOpaque Materials6 D1736 Test Method for Efflorescence of Interior Wall Paints4 D1737 Test Method for Elongation of Attached Organic Coatings with Cylindrical Mandrel Apparatus7 D1849 Test Method for Package Stability of Paint4 D2196 Test Methods for Rheological Properties of Non- Newtonian Materials by Rotational (Brookfield) Vis cometer4 D2243 Test Method for Freeze-Thaw Resistance of Wa ter-Borne Paints4 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates4 D 2369 Test Method for Volatile Content of Coatings4 D 2486 Test Method for Scrub Resistance of Interior Latex Flat Wall Paints4 ` D2574 Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms4 D2805 Test Method for Hiding Power of Paints by Reflectometry4 D 2831 Test Method for Evaluating the Ability of a Latex Paint to Resist Efflorescence from the Substrate8 D 3258 Test Method for Porosity of Paint Films4 D 3450 Test Method for Washability Properties of Interior Architectural Coatings4 D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings4 D 4062 Test Method for Leveling of Paints by Draw-Down Method4 D4213 Test Method for Wet Abrasion Resistance of Interior Paints4 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode9 E 105 Recommended Practice for Probability Sampling of Materials6 2.2 U. S. Federal Test Methods Standard 141:10 2112 Application by Roller 2131 Application of Sprayed Films 2141 Application of Brushed Films 6 Annual Book ofASTM Standards, Vol 14.02. 7 Discontinued; see 1988 Annual Book ofASTM Standards, Vol 06.01. 8 Discontinued, see 1980 Annual Bock ofASTM Standards, Part 27. ' 9'Amiidi Bookdf'ASTM'StdnddrdT, Voi 15,05'. 10 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 397 DU PO 502 97 578 C # D 2931 3011 Condition in Container TABLE 1 List of Test Methods by Properties 4321 Brush Properties 4541 Working Properties and Appearance of Dried Film 3. Definitions 3.1 For definition of terms used in this practice, refer to Definitions D 16 and D 1554. 4. Conditions Affecting Latex Wall Paints 4.1 Substrate Type--The substrate to be painted can affect not only the application properties and the physical properties of a latex paint, such as sheen and uniformity, but may also be a factor in determining the type of latex paint to Test Method Liquid Paint Properties: Condition in container Coarse particles and foreign matter Density (weight per gallon) Fineness of dispersion Odor Consistency (viscosity) Rheological properties, nonNewtonian liquids PH Color compatibility Section 7.1 7.2 7.3 7.4 7.5 7.S 7.7 7.8 7.9 ASTM Test Method Fe<iempf>\ 1 Method if Standaiw || Ho. I4i | D185 D 1475 D 1210 3011.1 I D562 0 2196 E 70 XSpiS'tlon application ^plicafo" Qpemioal a coarse par ^glorcornf color d>f,er instrume Color differ vi$ual & be used. For instance, a latex paint with good sealing properties may be required for porous surfaces, such as new dry wall, bare plaster, new wood or porous masonry surfaces. 4.2 Substrate Condition--Dirty, chalky, alkaline, or wa ter-soluble surfaces may affect tire practical requirements and performance of interior latex flat paints. 4.3 Application Properties--The application properties of interior latex paints are affected by temperature, humidity, and the texture and porosity of the surface to be painted. Application will also depend upon the type and quality of equipment used. 4.4 Physical Requirements--The type of latex wall paint to be used will depend not only upon the surface to be painted, but also upon the desired physical properties of the finish. For instance, if maximum light diffusion and unifor mity of appearance are the prime requirements, such as when painting ceilings, then a low sheen paint should be used. However, if cleanability or stain removal properties are desired for walls that become soiled, then a nonporous paint should be used. 5. Selection of Tests 5.1 It has been pointed out that there are many conditions that affect interior latex wall paints so that different types of latex paints have been developed specifically to meet the requirements of these various conditions. Although the recommended test methods presented in Tables 1 and 2 cover most of the properties of interior latex wall paints, all Freeze-thaw stability Package stability Microorganism resistance Paint Application and Film Formation: Application properties Application by brush Application by roller Application by spray equipment Drying time Flow and levelng Low-temperature coalescence of paints Producing uniform thickness of films Touch-up Appearance of Dry Paint Film: Color difference of opaque materials, visual evaluation Color difference of opaque materials, instrumental evaluation Hiding power Specular gloss Uniformity of appearance Properties of Dry Paint Film: Efflorescence of paint film Efflorescence from substrate Elongation (flexibility) Film porosity Scrubbabillty (wet abrasion) Stain removal {cleanability} Wet Abrasion Resistance Analysis of Paint: Chemical analysis Volatile content 7.10 7.11 7.12 8.1 8.1.1 8.1.2 8.1.3 8.2 8.3 8.4 8.5 8.8 9.1 9.2 9.3 9.4 9.5 10.1 10.2 10.3 10.4 10.5 10.6 10.7 11.1 11.2 D 2243 D1849 D 2574 ... D 1640 0 4062 D 3793 4541.49 , 2141.1 2112 2131 4061.1 I I$ 1 D 623 2162 D 1729 D 2244 D 344, D 2805 0 523 4541 D 1736 D2831 01737, D 522 D3258 D 2486 D 3450 D 4213 6221 6142 \ ? j . 1' | 1 I I I 1 | D 2369 rendition r consistent Density (w prying tin* Efflorescer Effloresce' Elongation Film poros Fineness t plow and Freeze-ths Hiding pot tow-temp pants Mieroorga Odor Package: pH producing Rheologic Newtor scrubbab specular Stain rem Touch-up Uniformity Volatile c> Wet Abra 1-gal tests, 1 Recon of these tests may not be required for each paint. If a paint is to be used only in a warm climate, for instance, then tant than others and specific values for each test cannot be 1 7- Liq fi freeze-thaw tests or low temperature coalescence tests need not be considered. 5.2 The purchaser should first determine which properties a latex paint must have and then select only those test methods that will measure or evaluate these properties. After selecting the desired tests, the purchaser should determine which of these properties are the most important and then establish the requirements or specifications of these tests to get the most desired properties. Since some paint properties recommended since the properties that are important to one purchaser may not be important to another. 6. Sampling 6.1 Prior to sampling, the condition of the container should be established since damage to it may cause evapora tion, skinning, or other undesirable effects in the coating. Determine the condition of the coating in accordance with 7.1 separa cannot stirrinj minin; mine Methc 7.2 tend to oppose each other, such as low sheen versus good 7.1 and 7.2. 7.2. cleanability, or high viscosity versus good leveling, some 6.2 Sample in accordance with Practice D 3925. Deter unifor properties may need to be attenuated if others are to be mine the weight per gallon in accordance with Test Method.. 2 weig accentuated. This balance of properties must be considered D 1475. Repeat this procedure until successive readings (45-fir when selecting the tests and establishing the requirements of agree within 0.2 lb (90 g) or as agreed upon between the of the; these tests. The properties that these tests measure and the purchaser and the seller. Samples for testing may then be and fc normal range of values have been presented,for many ofthe taken. - 7.2. tests, however. 6.3 Specify the amount of sample, the package sizes, and wheth 5.3 Some tests cannot be selected as being more impor- identification codes to assure a representative sample. A the su 398 DUP0502 97579 Federal Test Method Standard No. 141 3011.1 4541,4321 2141.1 2112 2131 4061.1 2162 4541 6221 6142 innot be it to one container evapora> coating, ince with 5. Detert Method readings ween the / then be sizes, and imple. A D2931 TABLE 2 Alphabetical List of Test Methods Test Methods Section ASTM Test Method Federal Test Method Standard No. 141 ^Application by brush Application properties Application by roller Application by spray equipment Chemical analysis Coarse particles and foreign matter Color compatibility Color difference of opaque materials, Instrumental evaluation Color difference of opaque materials, visual evaluation Condition in container Consistency (viscosity) Density (weight per gallon) prying time Efflorescence of paint film Efflorescence from substrate Elongation (flexibility) Hm porosity fineness of dispersion Flow and leveling Freeze-thaw stability Hiding power Low-temperature coalescence of paints Microorganism resistance Odor Package stability pH producing uniform thickness films Rheological properties of non- Newtonian liquids Scrubbability (wet abrasion) Specular gloss Stain removal (cleanability) Touch-up uniformity of appearance Volatile content Wet Abrasion Resistance 8.1.1 8.1 8.1.2 - 8.1.3 11.1 72 7.9 92 9.1 7.1 7.6 7,3 8.2 10.1 10.2 10.3 10.4 7.4 8.3 7.10 9.3 8.4 7.12 7.5 7.11 7.8 8.5 7.7 10.5 9.4 10.6 8.6 9.5 11.2 10.7 2141.1 4541, 4321 2112 2131 D 185 D 2244 D 1729 D 562 D1475 D1640 01736 D2631 D 1737, D522 0 3258 D 1210 04062 D2243 D344, D2805 D3793 3011.1 4061.1 6221 ... < D 2574 D1849 E70 D 623 D 2196 2162 D 2486 D 523 D 3450 D 2369 D4213 4541 1-gal (4-L) sample is usually sufficient-for the recommended tests, but for guidance in selecting a sampling plan, consult Recommended Practice E 105. 7. Liquid Paint Properties 7.1 Condition in Container--Thickening, settling, and separation are undesirable and objectionable if the paint cannot be reconditioned with a reasonable amount of stirring. The referenced method covers procedures for deter mining changes in properties of paints after storage. Deter mine the condition in the container in accordance with Method 3011 of Federal Test Method Standard No. 141. 7.2 Coarse Particles and Foreign Matter: 7.2.1 Paints must be free of coarse particles to form uniform films of good appearance, a typical maximum being 2 weight % of total paint. The specified test with a 325-mesh (45-um) screen and water as the wash liquid gives the percent of these particles in a latex paint. Determine coarse particles and foreign matter in accordance with Test Methods D 185. 7.2.2 Another test method used in industry to determine whether coarse particles are present in a dry film is to scrape the surface of the film with a spatula or metal edge of a ruler. Any particles larger than 325 mesh can be clearly seen after the surface has been scraped. 7.3 Density (Weight per Gallon)--The density as mea sured by weight per gallon (kilograms per litre) is used to assure product uniformity from batch to batch. It does not necessarily measure the quality of a paint. In the referenced method, the density is expressed as the weight in pounds of 1 U.S. gal (kg/L) of the paint at a specified temperature. Most interior flat latex, paints have densities of about 10 to 12 lb/gal (1.2 to 1.4 kg/L). Determine density in accordance with Test Method D 1475. 7.4 Fineness ofDispersion: 7.4.1 The more finely a pigment is dispersed, the more efficiently it is being used. One method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the material down a calibrated tapered groove varying in depth from 4 to 0 mils (100 to 0 pm). The point at which continuous groupings of particles or agglom erates, or both, protrude through the surface of the liquid is taken as the fineness reading. Lower readings in mils or micrometres or higher readings in Hegman units indicate better fineness of dispersion. 7.4.2 The referenced method was designed primarily for coatings with good fineness of dispersion, such as enamels. Most interior flat latex paints have finenesses of about 70 to 90 pm (1 to 2.5 Hegman). Although these paints may contain pigments so coarse that it is impractical to measure the fineness with a grind gage, most of the pigmehts are so finely dispersed that particles or agglomerates cannot be seen by the unaided eye or felt on the surface of the dry film. In addition, the fast drying of some flat latex paints may make it difficult to make accurate measurements of fineness of dispersion. 7.4.3 Determine fineness of dispersion with Test Method D 1210. 7.5 Odor--One of the advantages of latex paints is that they do not have odors characteristic of solvent-based coatings. However, other ingredients, such as ammonia, may be used which might also be objectionable in confined spaces. Thus, interior latex paints should be tested for odor acceptability. Although there is no adequate ASTM test method to measure odor for nonorganic solvent paints, test methods are used by industry to measure this property. Examine to determine if the paint has an unpleasant or irritating odor during application or drying. 7.6 Consistency (Viscosity)--Paints of a given type should fall within a stated consistency for satisfactory reproduction of a specific formula. While consistency is an important property it does not determine the quality of a paint and should be used mainly to assure product uniformity. In the referenced method, consistency is defined as the load in grams to produce a specified rate of shear. Although the consistency of most latex wall paint is about 150 to 300 g/100 revolutions, a much wider range is possible because of the wide variations in rheological properties of these paints. Also two paints of the same consistency may have quite different rheological properties. Determine the consistency in accordance with Test Method D 562. 7.7 Rheological Properties, Non-Newtonian Liquids-- Rheological properties are related to application and leveling properties of the liquid paint. The referenced method covers 399 DUP0502 97580 D 2931 the determination of rheological properties and i's particu larly suited for use with paints that display thixotropic characteristics. It actually measures viscosity under varying conditions of time and rotational speed of the spindle. Determine rheological properties in accordance with Test Methods D 2196. 7.8 pH--Latex paints with low (acidic) pH may corrode the container. pH may vary from about 5 to 10 depending upon the type of latex used and the general formulation. pH does not determine the quality of a latex paint and should only be used to assure product uniformity. A change in pH during storage may indicate poor stability or a change in properties of a latex paint. Determine pH in accordance with Test Method E 70. 7.9 Color Compatibility--A test method to determine how well colorants can be dispersed in a paint so that the paint will have uniformity of color when applied is now in preparation and will be included in this guide when adopted by ASTM. 7.10 Freeze-Thaw Stability--Water-based paints may be subjected to freezing conditions during shipping and storage. Suitably stabilized paints will resist several cycles of freezing and thawing without showing deleterious changes such as coagulation, graininess, or excessive viscosity increase. Many latex paints will increase in viscosity but can still be considered usable if other properties, which may be affected by a higher viscosity, such as leveling and brushability, are satisfactory. Determine freeze-thaw stability in accordance with Test Method D 2243. 7.11 Package Stability--Since paints cannot normally be used immediately after manufacture, they must remain stable in the can for some time. At normal temperatures, most latex paints can be stored for over a year with little change in properties. Although package stability can usually be determined in several weeks at an elevated temperature such as 122F (50C), occasionally the results of the acceler ated test do not coincide with those of prolonged room temperature storage. The referenced method covers the change in consistency and in certain other properties in packaged latex paint when stored at temperatures above freezing. Determine package stability in accordance with Test Method D 1849. 7.12 Microorganism Resistance--Bacteria in a latex paint can cause gassing, putrefactive, or fermentative odors and loss of viscosity. Determine if the paint contains living bacteria or ifit is resistant to attack by bacteria in accordance with Test Method D 2574.8 8. Paint Application and Film Formation 8.1 Application Properties--Determine the ease with which a paint can be applied to various wall surfaces with brush, roller, or spray equipment, in accordance with Method 4541 of Federal Test Method Standard 141. Appli cation properties are generally compared to a standard, or described by requirements in a product specification. 8.1.1 Brushing Properties--The specified method covers the determination of the brushing properties of coatings. The test is quite subjective although someone experienced in the art can produce quite consistent results, particularly in the evaluation of "drag" properties. Determine brushing proper ties in accordance with Method 4321 of Federal Test Methru jewing condi Standard No. 141. 0(5 4ures to be us< 8.1.2 Roller Application--Determine the ease with wfak 0{ opaque ma a paint can be roller applied in accordance with MethS apce with Prat 2112 of Federal Test Method Standard 141. Since roiw 9.2 Color D foam and roller spatter are often serious problems when law gvaluation--( paints are roller applied, these properties can also be deter standard can mined in the test method for roller application. The amoutJ tolerance is ag of foam produced, the time that it takes for the bubbles to may also be r< break, and the number of craters that remain after the although colo bubbles have broken can be determined by visual examina. eye, they pro tion of the test panel. Roller spatter can be determined bi quently comp placing a strip of paper or a panel at the bottom of the ter[ method covert panel to catch the paint spatters from the roller. The degr^ differences ol to which a paint will spatter when roller applied can ^ nonfluorescen determined by the density of the paint spatter. coated specim 8.1.3 Sprayed Film Application--Interior latex paints ate I ation (9.1) si sometimes applied by spray. Determine the spray application properties in accordance with Method 2131 of Federal Test Method Standard No. 141. The method can be modified to include application by airless spray equipment. instrumental r with Method 9.3 Hiding measure of tb 8.2 Drying Time--The drying time of an interior latex however, dep' paint is important in determining when a freshly painted influenced by room can be put back to use. Under average conditions most practical test fiat latex paints are dry to touch in 1 or 2 h when the water thickness is has evaporated from the film. They can usually be recoated visually as cc from within a few hours to 18 h. Curing to obtain the affected by fl ultimate properties may take only a few days for some late* paints while others may require 1 or 2 weeks depending upon the composition. Determine drying time in accordance with Test Methods D 1640. paint. Test f precise and at standard. Pah the effects of 8.3 Flow and Leveling--These properties are usually measured, ar evaluated by visually examining the test panel after a paint mine hiding ] has been applied by brush or roller to see if any brush or or D 2805. roller marks can be seen in the dry film. Determine the 9.4 Specul ability of the paint to flow out after application in accord 85 geometr ance with Test Method D 4062. appearance o 8.4 Low-Temperature Coalescence of Paints--Determine ; 85 sheen ol how well the latex particles in a paint will fuse together or : uniformity of coalesce, to form a continuous film at low temperatures in 1 paints with accordance with Test Method D 4062. , sheen, this i 8.5 Producing Films of Uniform Thickness--The fol i should not 1 lowing method covers the preparation of various films of t Determine t uniform thickness essential in conducting tests. Prepare films D 523. in accordance with Test Methods D 823. 9.5 Unifo 8.6 Tpuch-Up--Although there is no test method pub I Method 45^ lished in Federal Test Method Standard 141 to measure I examine the touch-up, test methods are used by . the paint industry. The I color or shee usual method is to apply the test paint to a small section ofa test panel that has previously been painted with the test paint I 10. Properti and allowed to dry.,The touch-up area is usually applied with | 10.1 Efflo a small brush. When the touch-up area has dried, it is : method mea examined to see if there is any difference in color or sheen itself, not f: between the touched-up area and the initial coat of paint. effloresce dt . I I.' j formulations 9. Appearance of Dry Film* \ tions of ter 9.1 Color Differences of Opaque Materials by Vised 1 sufficient sol Evaluation--Visual comparison of color is fast and often deposit on t acceptable although numerical values are not obtained. The : accordance \ referenced method covers the spectral, photometric, and geometric characteristics of fight source, illuminating and 10.2 Efflo strates may c 400 DU P0502 97581 D2931 Test Method : with which /ith Method Since roller s when latex so be deterThe amount ' bubbles to in after the al examina:ermined by a of the test The degree lied can be x paints are application 'ederal Test modified to iterior latex hly painted litions most n the water be recoated obtain the some latex depending accordance tre usually fter a paint :y brush or ermine the in accord- -Determine together or "ratures in -The fols films of pare films :hod pubo measure lustry. The action of a e test paint pplied with iried, it is )r or sheen of paint. by Visual and often ained. The letric, and rating and viewing conditions, size of specimens, and general proce dures to be used in the visual evaluation of color differences of opaque materials. Determine color difference in accord ance with Practice D 1729. 9.2 Color Differences ofOpaque Material by Instrumental Evaluation--Color difference between a product and the standard can be measured by instrument. Generally, the tolerance is agreed upon by the purchaser and the seller and may also be required if a product specification is involved. Although color instruments are not more sensitive than the eye, they provide numerical values which can be subse quently compared to later measurements. The referenced method covers the instrumental determination of small color differences observable in daylight illumination between nonfluorescent, nonmetameric, opaque surfaces such as coated specimens. If metamerism is suspected, visual evalu ation (9.1) should be used to verify the results. Make instrumental measurement of color difference in accordance with Method D 2244. 9.3 Hiding Power (Dry Opacity)--Hiding power is the measure of the ability of a paint to hide the substrate. It is, however, dependent upon uniform film thickness which is influenced by flow and leveling. Test Method D 344 is a practical test in which paint is applied with a brush, film thickness is approximately measured, opacity is evaluated visually as compared to a standard paint, and results are affected by flow and leveling application properties of the paint. Test Method D 2805 is considered to be a more precise and accurate test that does not need a material paint standard. Paint is applied with an applicator bar to minimize the effects of flow and leveling, film thickness is rigorously measured, and opacity is instrumentally evaluated. Deter mine hiding power in accordance with Test Methods D 344 or D 2805. 9.4 Specular Gloss (Sheen)--The method given, using the 85 geometry, is useful in characterizing the low angle appearance of flat paints. Most flat latex wall paints have an 85 sheen of about 1 to 10. Although paints with good uniformity ofappearance are often paints oflower sheen and paints with good cleanability are often ones with higher sheen, this is not always the case, and the sheen of a paint should not be used as a measure of other paint properties. Determine the 85 gloss in accordance with Test Method D523. 9.5 Uniformity of Appearance--Apply the paint as in Method 4541, Federal Test Method Standard 141, and examine the dry paint to see if there is any nonuniformity of color or sheen. 10. Properties of Dry Film 10.1 Efflorescence of the Paint Film--The referenced method measures efflorescence that comes from the paint itself, not from the substrate. Few interior latex paints effloresce due to improvements in latex and latex paint formulations. Salt formation is produced by specific condi! tions of temperature and. humidity if a paint contains sufficient solid water-soluble material to cause a noticeable deposit on the film. Determine efflorescence resistance in accordance with Test Method D 1736. 10.2 Efflorescence from Substrate--Cementitious subj strates may contain sufficient solid water-soluble materials to cause a surface deposit through leaching and evaporation. Determine if a latex paint applied over an alkaline masonry surface will allow soluble salts to pass through the film in accordance with Test Method D 2831. 10.3 Elongation--Elongation is a measure of the flexi bility of a paint film. Most interior latex paints can be bent over a 'A in. (6.4-mm) mandrel without affecting the film. Determine elongation in accordance with Test Methods D 522 or D 1737. 10.4 Film Porosity--The more porous a paint is, the worse will be its cleanability and enamel holdout. Determine the film porosity in accordance with Test Method D 3258. 10.5 Scrubbability--The ability of an interior finish to resist scrubbing is an important property. The referenced method provides a measure of the wet abrasion resistance of a film. However, wet abrasion resistance is not necessarily a measure of how well soils or stains can be removed since some paints have good scrubbability but poor stain cleanability because they are porous. The scrubbability of interior latex flat paints can vary from less than 100 to more than 1000 cycles. Determine the scrubbability in accordance with Test Method D 2486. A control paint should always be tested at the same time because of the variability of the method. 10.6 Stain Removal (Cleanability)--The ability to re move marks satisfactorily without damaging the film is an important property of interior finishes. A test method to determine how well stains and soils can be removed from a cured paint film is now in preparation and will be included in this guide when it is approved by ASTM. Test methods used by the paint industry consist of applying various household soils or stains to the cured paint film and attempting to remove these soils or stains by means of a washing or scrubbing operation. The attempted removal of the soils or stains can be done by hand or with a mechanical apparatus. Determine the relative ease of removal of soil from the dried film by washing with either an abrasive or nonabrasive cleaner in accordance with Test Method D 3450. 10.7 Wet Abrasion Resistance (Weight Loss Method)-- This method differs from Test Method D2486, scrub resistance (10.5), in that the loss in weight or volume of the paint film is recorded for each 100 scrub cycles. In Test Method D 2486 the number of scrub cycles required to wear through the paint film is recorded. Determine the wet abrasion resistance of the paint in accordance with Test Method D 4213. 11. Analysis of Paint 11.1 Chemical Analysis--If a specification requires cer tain raw materials or certain components in a given amount, then chemical analysis is required to determine whether the specified materials are present and in what amounts. Anal ysis does not necessarily establish paint quality which can also be greatly affected by manufacturing techniques. Most ASTM analytical methods apply to solvent-based coatings. However, some of them can be adapted for analysis oflatex paints. 11.2 Volatile Content--The amount of volatile material in a paint cannot be used as an indication of the quality of a paint. This value is useful, however, in determining the 401 DUP050297582 W > 2931 similarity df two samples. Determine volatile content in accordance with Test Method D 2369. 12. Field Testing 12.1 Although the recommended test methods attempt to duplicate actual conditions under which latex flat wall paj are applied, it is not possible to duplicate all ppssihf conditions. It is therefore necessary to test latex flat paints under actual existing conditions for a final evaluati of the quality of a paint. 0j j The American Society for Testing and Materials takes noposition respecting the validity ofany patentrights asserted in connection with any item mentioned in this standard,. Users of this standard are expressly advised that determination oI the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapprovedor withdrawn. Your comments are invited either for revision ofthis standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive Careful consideration at a meeting of the responsible technical committee, which you may attend. If you teeI that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia PA 19103. 1 1. s 1. k i for coat incl not to 1 reqi me] 1 red bru an> 1 noi use ;a 1 ,!r res sur wb is i S' 33 ;! ; Slg', i [ M\ cdi : : ' os... 4\ i ii! I ,1: | i.-lf-j f ..4| ,3^1 i , : ino|; . -.Mil l all res Fc tri ti< u; cc a. at tk ai a] 2. 402 DUR050297583 Designation: D 2932 - 80 (Reapproved 1988)'['*1 Standard Guide for Testing Exterior Solvent-Reducible House and Trim Coatings1 This standard is issued under the fixed designation D 2932; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (6) indicates an editorial change since the last revision or reapproval; 1 N' --Editorial changes were made throughout, including the title, in October 1988. j. Scope 1.1 This guide covers the selection and use of procedures for testing exterior solvent-reducible house paints and trim coatings in the laboratory and in the field. The test methods included are listed in Tables 1 and 2. All of these tests may not be required for each paint Selection of the test methods to be followed must be governed by experience and the requirements in each individual case, together with agree ment between the purchaser and the seller. 1.2 This guide covers the testing of ready-mixed solventreducible house paint or trim coatings for application by brush, roller, or spray on exterior surfaces: The paint may be any of the following types: 1.2.1 Type I Paint, Oil--Titanium, lead, zinc, and oil, nonfume-resistant, white and colors. For general exterior use, particularly on wooden structures. 1.2.2 Type II Paint, Oil--Titanium, zinc, and oil, fumeresistant, white and colors. Suitable for use on exterior surfaces such as wood and primed steel or sealed concrete, where resistance against discoloration from hydrogen sulfide is required. 1.2.3 Type III Paint, Oil-Alkyd--Combination of oil and alkyd in the vehicle and pigments, composed of chalkresistant and chalking titanium dioxide, white and colors. For general exterior use, particularly on wooden surfaces, trim, primed steel, or sealed concrete. 1.2.4 Type IV Paint, Miscellaneous Vehicles-^Comhin^tion of pigments and vehicle, white and colors. Suitable for use on exterior wooden surfaces, trim, primed Steel, or sealed concrete. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents- 2.1 ASTM Standards: D16 Definitions of Terms Relating to Paint, Varnish, Lacquer, and Related Products2 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester3 D154 Guide for Testing Varnishes4 D.185 Test Methods for Coarse Particles in Pigments, Pastes, and Painty5 D 215 Methods of Chemical Analysis of White Linseed Oil Paints4 D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts4 D358 Specification for Wood to Be Used as Panels in Weathering Tests of Coatings4 D522 Test Method for Mandrel Bend Test of Attached Organic Coatings4 D523 Test Method for Specular Gloss4 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer4 D659 Method of Evaluating Degree of Chalking of Exterior Paints4 D 660 Test Method for Evaluating Degree of Checking of Exterior Paints4 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints4 D 662 Test Method for Evaluating Degree of Erosion of Exterior Paints4 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints4 D1006 Practice for Conducting Exterior Exposure Tests of Paints on Wood4 D1038 Definitions of Terms Relating to Veneer and Plywood6 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems4 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products4 D1554 Definitions of Terms Relating to Wood-Base Fiber and Particle Panel Materials6 D1640 Test Methods for Drying, Curing, or Filin Forma tion of Organic Coatings at RooiriTemperature4 D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials7 Dl737'Test Method for Elongatidh of Attached Organic Coatings with Cylindrical Mandrel Apparatus81 1 This practioe isimder the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials, and is die direct responsibility of Subcommittee D01.42 on Architectural Finishes. __ - ........... ... Current edition approvecTAug. I, 198(3. Published November 1980. Originally published as D 2932 - 70 T. Last previous edition D 2932 - 7$^ 2 Annual Book ofASTM Standards, Vols 06.01, 06.02, and' 06.03. 3 Annual Book ofASTM Standards, Vols 05.01, 06.01, and 06.03. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vote 06.01 and. 06.02. 6 Annual Book ofASTM Standards, Vol 04.09. 7 Annual Book ofASTM Standards, Vol 14.02. 8 Discontinued; see Annual Book ofASTM Standards. Vol 06.01. 403 DUP050297584 # D 2932 Si D2196 Test Methods for Rheological Properties of Non- Newtonian Materials by Rotational (Brookfield) Viscometer4 D2244 Test Method for Calculation of Color Differences From Instrumentally Measured Color Coordinates4 D2245 Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints8 D 2366 Test Method for Accelerated Testing and Moisture Blister Resistance of Exterior House Paints on Wood7 D 2369 Test Method for Volatile Content of Coatings4 D2371 Test Method for Pigment Content of Solvent- Reducible Paints4 D2372 Method of Separation of Vehicle from Solvent- Reducible Paints4 D2621 Test Method for Infrared Identification of Vehicle Solids from Solvent-Reducible Paints4 D2698 Method for Determination ofthe Pigment Content of Solvent-Reducible Paints by High-Speed Centri fuging4 D2805 Test Method for Hiding Power of Paints by Reflectometry4 . D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus9 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry10 E 105 Recommended Practice for Probability Sampling of Materials7 2.2 U. S. Federal Test Method Standard 141:u 141/1021 Sampling (General) 141/2131 Application of Sprayed Films 141/2141.1 Application of Brushed Films 141/3011.1 Condition in Container 141/4203.1 Reducibility and Dilution Stability 141/4421 Absorption Test 141/4541 Working Properties and Appearance of Dried Film 3. Definitions 3.1 For definition of terms used in these practices, refer to Definitions D 16, D 1554, and D 1038. 4. Conditions Affecting Solvent-Based House and Trim Coatings 4.1 Practical requirements and performance for solvent house or trim paints may vary with: 4.1.1 Substrate type, such as type and quality of wood or hardboard; type of grain of wood; knots; and type, quality, and alkalinity of concrete substrates. 4.1.2 Condition of previously painted substrates such as degree of chalk, adhesion of film, dirt, mold, and general condition of old coating, 4.1.3 Type and quality of primer and time before topcoating, 4.1.4 Climatic conditions at the time of coating applica tion and immediately after application, 5 Annual Book ofASTM Standards, Vol 06.03. 10 Annual Book ofASTM Standards. Vols 06.01 and 14.02. 11 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 200 Robbins Ave-, Philadelphia. PA 19111-5094. TABLE 1 List of Test Methods by Properties Test Method Section ASTM Test Method Liquid paint properties: Skinning Condition in container Coarse particles and foreign matter Weight per gallon or density Fineness of dispersion Consistency Dilution stability Rheological properties of non-Newtonian liquids Absorption Flash point 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.6 6.9 6.10 Paint application and Dim formation: Working properties Application by brush Application by spray Drying properties 7.1 7.2 7.3 7,4 D 154 D185 D 1475 D 1210 0 562 D 2196 0 93, D 3278 D 1640 3021 4091 ' 41841 .ft n 4411.! 4281 4203.1 fe P 4421 flr? sy 4541 P 2141.1 2131 f Up 4061.1/j ADS APP APP Cria Cfie Che Coe in cok Con EXte ConCrac Dire* OW oryti Elbn Appearance of dry paint film: Color difference of opaque materials. visual evaluation of Color difference of opaque materials. instrumental evaluation of Directional reflectance Gloss (60-dsg specular) Hiding power Properties of dry paint film: Elongation (flexibility) Moisture blister resistance Fume resistance Exterior exposure resistance Wood panel description Chalk resistance ratings Checking resistance ratings Cracking resistance ratings Erosion resistance ratings Flaking resistance ratings Analysis of paint: Chemical analysis Volatile content Pigment content Pigment analysis Nonvolatile vehicle content Identification of vehicle solids Identification of oils 8.1 8.2 8.3 8.4 8.5 v 9.1 9.2 9.3 9.4 9.4.1 9.4.2 9.4.3 9.4.4 9.4.5 9.4.6 10.1 10.2 10.3 10.4 10.5 10.6 10.7 D 1729 D 2244 E 97 D 523 D 2805 D 344 D1737 D 2366, D 522 D 1006 D 358 0 659 D 660 D 661 D 662 D772 D215 0 2369 0 2371, D 2696 D215 D215 02621 0 2245 Pv 4249.lt t1 61230^8 6121*^? 6131*1 4121 IS * jp ' 4$ r 622lil f 1 8161.15 2031, ijj 6411; 0 6421JJ i 6471*1 t 64318# 6441;$|! z "'1 1 i .. 4041ill| 4Hi| .,J1 & 7261,6i 4059 4 1 75M P Eros Fine Flak Fiasi r Fum Hidlr Wen- Mois Nom Pigm Pigrr Rhe< liq Sam1 Skim Votai Weig Woo --Wof 1 ` t san k rail acc the 0.11 1 4.1.5 Environmental conditions after application/ ml general for the area and specific, such as under eaves, bei shrubbery, and north- and south-side exposures, and 4.1.6 Structural aspects of the building. If constructionH I defects due to age are such that excessive moisture | inside or from the outside makes its way through to, substrate, blistering, flaking, or peeling may result. 5 ider 5. Sampling 5.1 To ensure an adequate and representative sample! paint to conduct tests agreed upon between the pure! and the seller, proper sampling is important. - , 5.2 Sample the coating in accordance with Method1) of U. S. Federal Test Method Standard 141. Prior 404 DUP0502 97585 Federal ~~ Teat Method Std. No. 141 -- 3021 3011.1 4091 4184.1 4411.1 4281 4203.1 4421 4541 2141.1 2131 4061.1 4249.1 6123 6121 6101 4121 6221 6161.1 2031 6411 6421 6471 6431 6441 1041.1 021.1 261 053 501 n, both . behind ction or rom the i to the mple of jrchaser :d 1021 hior to D2932 TABLE 2 Alphabetical List of Test Methods Test Method Section ASTM Test Method absorption Application by brush Application by spray Chalk resistance ratings Checking resistance ratings Chemical analysis Coarse particles and foreign matter Color difference of opaque materials, instrumental evaluation of Color difference of opaque materials, visual evaluation of Condition in container Exterior exposure resistance Consistency viscosity Cracking resistance ratings Directional reflectance Dilution stability Drying properties Elongation (flexibility) Erosion resistance ratings Fineness of dispersion Flaking resistance ratings Flash point Fume resistance Gloss (60-deg specular) Hiding power identification of oils Identification of vehicle solids Moisture blister resistance Nonvolatile vehicle content Pigment analysis Pigment content Rheological properties of non-Newtonian liquids Sampling Skinning Volatile content Weight per gallon or density Wood panel description Working properties 6.8 7.2 7.3 9.4.2 9.4.3 10.1 6.3 8.2 D6S9 D660 D 215 D 185 0 2244 8.1 D1729 62 9.4 6.6 9.4.4 8.3 6.7 7.4 9.1 9.4.5 6.5 9.4.6 6.10 9.3 8.4 8.5 10.7 10.6 9.2 10.5 10.4 10.3 6.8 0 1006 0 562 D 66t E 97 D 1640 D1737, O 522 D662 D1210 D772 D93, D 3278 D 523 D 2805, D344 D2245 O 2621 D2366 D215 D215 D2371, D 2698 D2196 5 6.1 10.2 6.4 9.4.1 7.1 0154 D2369 D1475 D358 Federal Test Method Standard No. 141 4421 2141.1 2131 6411 6421 4091 6123 4249.1 3011.1 6161.1 4201 6471 612V 4203.1 4061.1 6221 6431 4411.1 6441 6101 4121 7501 4053 7261 4021.1 1021 3021 4041.1 4184.1 2031 4541 sampling, stir the paint as in 4.21 of Method 1021. Deter mine the weight per gallon (or kilograms per litre) in accordance with Test Method D 1475. Stir again and recheck the weight per gallon. The two readings should agree within 0.10 lb (45 g). 5.3 Specify the amount of sample, the package sizes, and identification codes to assure a representative sample. A 1-gal (4-L) sample is usually sufficient for the recommended tests but for guidance in selecting a sampling plan consult Recommended Practice E 105. 6. Liquid Paint Properties 6.1 Skinning--Paints containing a binder, that dries by oxidation are subject to skin formation in a partially filled can or by diffusion of air into the can. Since skins are insoluble in the paint, they must be removed before use. This test in a partially filled container indicates the tendency of a paint to skin. Examine the original sample for skins, both on the surface and in its mass. Using a well-mixed, skin-free portion of the sample, perform a skinning test in accordance with Guide D 154. No t e 1--A typical minimum time for skinning in accordance with Guide D 154 is 48 h. 6.2 Condition in Container--After storage, paints should be suitable for application with minimum stirring. Charac teristics that are undesirable and objectionable in a stored paint are given in the referenced test method. Determine condition in container in accordance with Method 3011.1 of Federal Test Method Standard No. 141. 6.3 Coarse Particles and Foreign Matter~ Paints must be free of oversize particles and foreign matter to form a uniform film of good appearance. This test, with a 325-mesh (45-|xm) screen, gives the percent of these particles in the paint. Determine coarse particles and foreign matter in accordance with Test Methods D 185. No t e 2--A typical maximum for coarse particles and foreign matter is 1 weight % of total paint. 6.4 Density or Weight per Gallon--The density of a paint as measured by weight per gallon (or kilograms per litre) provides a check against the theoretical weight calculated from the formula and is useful for determining similarity of two samples. The density is expressed as the weight in pounds of 1 U. S. gal (or kilograms per litre) of the liquid at a specified temperature. A calibrated weight per gallon cup is used. Determine weight per gallon in accordance with Test Method D 1475. 6.5 Fineness ofDispersion--The more finely a pigment is dispersed the more efficiently it is being utilized. One method for measuring degree of dispersion is to draw a paint down a tapered groove in a hardened steel block with the groove varying in depth from 4 to 0 mils ((100 to 0 pm) 0-8 Hegman units). The point at which continuous groupings of particles or agglomerates protrude through the surface of the wet film is taken as the dispersion reading. Higher readings (Hegman units) indicate better dispersion. Determine the fineness of dispersion in accordance with Test Method D 1210. N' 3--A typical reading for house paint is 60 pm (approximately 2'/2 mils) and for trim paint 25 pm (1 mil). Several arbitrary, scales and modifications of the gage are used by industry. The approximate relationship of these scales to micrometre and mil readings is shown in Test Method D 1210. 6.6 Consistency (Viscosity)--Paints of a given type should fall within a stated consistency range for satisfactory repro duction of a specific formula. While consistency is an important property, it does not determine the quality of a paint and should be used mainly to assure product uni formity. In the referenced method consistency is defined as the load in grams to produce a specified rate of shear. Although the consistency , of most solvent-based house and trim coatings is about 150 to 300 g/100 revolutions, a much wider range is possible because of the wide variations in rheological properties of these paints. Also two. paints of the same consistency may have quite different rheological prop erties. Determine the consistency in accordance with Test Method D 562. 6.7 Dilution Stability--Dilution with a specified thinner shows whether the materials are compatible and whether the reduced paint is stable. The referenced test is a measure of 405 DU P050297586 >1 nk, "S IS D2932 the stability of paint that has been reduced to a desired viscosity, for example, for spray application. The diluent suggested for reduction should be readily incorporated into the paint without excessive stirring or shaking. Determine dilution stability in accordance with Method 4203 of Federal Test Method Standard No. 141. 6.8 Rheological Properties of Non-Newtonian Liquids-- Rheological properties are related to application and flow properties of the liquid coating. The referenced test method covers the determination of the rheological properties of a paint and is particularly suited for use with paints that display thixotropic characteristics. It actually measures vis cosity under varying conditions of time and rotational speed of the spindle. Determine rheological properties in accord ance with Test Methods D 2196. 6.9 Absorption--On porous surfaces, binder penetration can result in pigment volume concentration changes as the film dries. This may cause performance to vary. The referenced method provides a rapid means for measuring the relative penetration of the binder into a porous surface. It provides a rough measure of the wetting and penetrating, quality of liquid materials. Determine the absorption in accordance with Federal Test Method Standard No. 141, Method 4421. 6.10 Flash Point--When the flash point of a material is required for shipping information, use Test Methods D 93, Part B, or D 3278. 7. Paint Application and Film Formation 7.1 Working Properties--Working properties of a paint are generally compared to a standard or described by requirements in the product specification. Test working properties in accordance with Method 4541 of Federal Test Method Standard No. 141. 7.2 Application by Brush--Brushed films should be smooth and free of seeds and on vertical surfaces should show no sagging, streaking, or excessive brush marks. For proper method of application of a brushed film for test purposes, refer to Method 2141.1 of Federal Test Method Standard No. 141. 7.3 Application by Spray--This method covers applica tion of a paint by spray, which is sometimes used for house and trim paint. Refer to Method 2131 of Federal Test Method Standard No. 141. 7.4 Drying Properties--The drying time of a coating is determined by its composition and by atmospheric condi tions during drying. Insufficient, drying may result in dirt or insect pickup resulting in a poor appearance, or a nonuniform appearance caused by dew or rain falling on the paint film. Testing a paint for the required drying properties can determine whether the paint has lost its drying properties through aging or whether insufficient drier was included in the product at the time of manufacture. The specific category, of drying should be selected to suit the types of house paint being tested, since drying times vary widely. Determine the drying time in accordance with Test Methods D 1640. 3. Appearance of Dry Paint Film 8.1 Color Difference of Opaque Materials, Visual Evalua tion of-- Visual comparison is fast and often acceptable although numerical values are not obtained. The referenced practice covers the spectral, photometric, and geometry characteristics of light source, illuminating and viewing conditions, sizes of specimens, and general procedures to bj used in the visual evaluation of color differences of opaque materials. Determine the color difference in accordance with Practice D 1729. 8.2 Color Difference of Opaque Materials, Instrument Evaluation of--Color difference between a product and the standard can be tested by instrument. Generally the toler, ance is agreed upon between the purchaser and the seller and may also be required if a product specification h involved. Determine the color difference in accordance with Method D 2244. 8.3 Directional Reflectance--This property is a measure of light reflected from the surface of the paint. It usually is assigned a value in specifications for white and pastel shades. Determine daylight directional reflectance in accordance with Test Method E 97. 8.4 Gloss _ (60-deg Specular)--Determine the specular gloss in accordance with Test Method D 523. Oil house paints are typically in a gloss range from 30 to 70, while trim enamels are in a gloss range from 70 to 90. 8.5 Hiding Power (Dry Opacity)--Hiding power is the measure of the ability of a paint to hide the substrate. It is, however, dependent upon uniform film thickness which is influenced by the flow and leveling. Test Method D 344 is a practical test in which paint is applied with, a brush, film thickness is approximately measured, opacity is evaluated visually as compared to a standard paint, and results sire affected by flow and leveling application properties of the paint Test Method D 2805 is considered to be a more precise and accurate test that does not need a riiaterial paint standard. Paint is applied with an applicator bar to minimize the effects of flow and leveling, film thickness is rigorously measured, and opacity is instrumentally evaluated. Deter mine hiding power in accordance with Test Methods D 344 or D 2805. 9. Properties of Dry Paint Film 9.1 Elongation (Flexibility)--Elongation is a measure of flexibility of a paint film. Generally, gloss house paints and trim paints will have no problem in passing a mandrel bend test. Flat house paints, however, may fail a sharp bend. Determine elongation in accordance with Test Methods D 1737 dr D 522. 9.2 Moisture Blister Resistance--Blister resistance is re lated to the ability of a dry paint film to resist the formation of blisters caused by water from the wood substrate. The watercan come from either the interior of the home or from structural defects that permit entry of the water behind the wood. Moisture blister resistance can be qualitatively evalu: ated in a laboratory test. Determine resistance to moisture blistering in accordance with Test Method D2366. 9.3 Fume Resistance--Fume resistance is the ability of a dry paint film to resist discoloration in a moist hydrogen sulfide atmosphere. This type of atmosphere may be present near industrial or other polluted areas and can cause paint to yellow or darken in as little time as overnight exposure. There are no ASTM or Federal test methods for evaluating1 this property, but one procedure used by the industry is as follows: 9.3. two g for 6 i hydro unext darke note paint oxide for d: 9.4 terioj 9A perfc D 35 9.` tan 9.> resis 9, resis 9. sista 9. sista 10. 1' cifi< test 406 DUPO 50297587 D2932 ,d geometric and viewjn ;edures to ^ es of opaq ordance ! ; 9.3.1 Apply a sufficient number of coats of the paint to glass plates to hide the surface completely, allow to dry L. 6 h and expose one of the plates in a moist atmosphere of Llrogen sulfide for 18 h.. Compare the color with the ^exposed plate. The exposed plate should be practically no wker than the unexposed one, The color difference should Instrument duct and the lly the to]er? id the selier xification jj ardance ot exceed that between plates that have been coated with a oJint made with titanium dioxide pigment, lead-free zinc Jjjdde, raw or refined linseed oil, and sufficient cobalt added for drying, and which has been similarly treated. 9.4 Exterior Exposure Resistance--In conducting ex- terjor exposures, refer to Practice D 1006. 9.4.1 Wood Panel Description--In establishing exposure is a measure It usually js >astel shades accordance performance, use the panels as described in Specification D358. 9.4.2 Chalk-Resistance Ratings--Determine chalk-resis tance rating using Method D 659. 9.4.3 Checking-Resistance Ratings--Determine checking- :he specular h Oil house 0, while trim resistance rating using Method D 660. 9.4.4 Cracking-Resistance Ratings--Determine cracking- resistance rating using Test Method D 661. ,. 9.4.5 Erosion-Resistance Ratings--Determine erosion-re lower is the bstrate. It is, ess which is sistance rating using Test Method D 662. 9.4.6 Flaking-Resistance Ratings--Determine flaking-re- sistance rating using Test Method D 772. d D 344 is a brush, film 10. Analysis of Paint is evaluated 1 results are erties of the be a more 10.1 Chemical Analysis--If a specification requires spe cific ingredients, chemical analysis may be required. Select test procedures from Methods D215, and other ASTM methods that are pertinent to the components of exterior house paints. < No t e 5--No single schematic analysis is comprehensive enough to cover the wide variety of house paint compositions. 10.2 Volatile Content--Thinner is removed from the paint at 110C. The percentage of volatile matter calculated from this loss in weight indicates the thinner loss from the film as the paint dries. Determine volatile content of the paint in accordance with Test Method D 2369. 10.3 Pigment Content--The pigment gives paint its hiding arid color and influences many other properties of the paint. Determine the percent pigment in accordance with Test Method D 2371. 10.4 Pigment Analysis--The analysis of pigment may be required if the product is covered by a specification, or upon agreement between the purchaser and the seller. Determine analysis of pigments in accordance with the selected test procedure from Method D 215. 10.5 Nonvolatile Vehicle Content--The nonvolatile ve hicle; is that portion of the film-forming solids in a paint other than the pigment Water, volatile thinner, and pigment are determined and the sum subtracted from the total weight to give the nonvolatile vehicle content. Determine the nonvolatile vehicle content in accordance with Method D215. Separate the vehicle for further analysis in accord ance with Method D 2372. 10.6 Identification of Vehicle Solids--Determine identity of vehicle solids in accordance with Methods D 2621. 10.7 Identification ofOils--Determine identity of oils in accordance with Methods D 2245. iaterial paint to minimize The American Society tor Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ot any such is rigorously patent rights, and the risk of infringement ot such rights, are entirely their own responsibility. ated. Deterhods D 344 This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and It not revised, eitherreapproved or withdrawn. Your comments are Invitedeither for revision ofthis standard or toradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feat that your comments have nut received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. measure of paints and .ndrel bend harp bend, t Methods :ance is reie formation bstrate. The mie or from behind the tively evaluto moisture 66. 5 ability of a st hydrogen y be present luse paint to it exposure. >r evaluating idustry is as DU P050297588 Last ASTM Designation: D 2933 - 74 (Reapproved 1986)61 Standard Test Method for Corrosion Resistance of Coated Steel Specimens (Cyclic Method) This test method is intended for use in determining the resistance to failure of coatings of paint, varnish, lacquer, and related products on steel surfaces when exposed cyclically to salt spray, humidity, and cold to induce coating failure more representative of the type found in outdoor corrosive environments. Formerly under the jurisdiction of Committee D-l on Paint and Related Coatings and Materials, this test method was discontinued in 1992. 1. S 1. and rigic cove 1. alio add the app app 2. 1 2 E E E E E E E r i i i i i < Reli D01 ( pub i 408 DUP0502 97589 Designation: D 3002 - 81 (Reapproved 1987) Standard Practice for Evaluation of Coatings for Plastics1 This standard is issued under the fixed designation D 3002; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. j. Scope 1.1 This practice is intended for the evaluation of clear and pigmented coatings designed for use on rigid or semi rigid plastic substrates. Coated film and sheeting are not covered by this practice. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. * 1. Referenced Documents 2.1 ASTM Standards: D 523 Test Method for Specular Gloss2 D658 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive2 D968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive2 D1308 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes2 D1474 Test Methods for Mentation Hardness of Organic Coatings2 D1544 Test Method for Color of Transparent Liquids {Gardner Color Scale)3 D1644 Test Methods for Nonvolatile Content of Varnishes2 D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials4 ' D2091 Test Method for Print Resistance of Lacquers2' D2199 Test Method for Measurement of Plasticizer Mi gration from Vinyl Fabrics to Lacquers2 D 2244 Test Method for Calculation of Color Differences From Instrumentally Measured Color Coordinates2 D2246 Test Method for Finishes on Primed Metallic Substrates for Humidity-Thermal Cycle Cracking2 D2247 Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity2 D 3170 Test Method for Chipping Resistance of Coatings2 D 3359 Test Methods for Measuring Adhesion by Tape Test2 G24 Practice for Conducting Natural Light Exposures Under Glass4 1 This practice is under the jurisdiction ofASTM Committee D-l on Paint, and Related Coatings and Materials and is the direct responsibility of Subcommittee EX)1.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Oct. 30, 1981. Published December 1981. Originally published as D 3002 - 71. Last previous edition D 3002 - 78. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 4 Annual Book ofASTM Standards, Vol 14.02. 3. Significance and Use 3.1 This practice is designed to set up a series of screening tests that will indicate the performance level to be expected of a coating or coating system on a given plastic substrate. 3.2 Rigid and semirigid plastic substrates vary widely in their acceptance characteristics for a given coating. 3.3 Surface cleaning or preparation prior to application of the coating can be critical to the proper performance of the coating. - 4. Precaution 4.1 This standard may involve the use of hazardous materials, operations, and equipment. It is the responsibility of whoever uses this standard to establish appropriate safety practices and to determine the applicability of regulatory limitations prior to use. 5. Test Panels and Panel Preparation 5.1 Unless directed otherwise, conduct performance tests on coatings of specified thickness applied to a normally molded sample of the designated plastic. Applied coatings cannot correct surface defects from improper molding proce dures. 5.2 Preparation of test samples shall include any cleaning, metalizing, or priming operations agreed, upon by the producer and the user. 5.3 Air-dry or bake the system according to the estab lished schedule and aged as agreed between the producer and the user. 6. Nonvolatile Matter 6.1 Test for nonvolatile matter in the coating material in accordance with Test Methods D 1644. 7. Color 7.1 Clear (on liquid sample)--Determine the Gardner color in accordance with Test Method D 1544. 7.2 Pigmented (on dry film)--Evaluate color differences visually in accordance with Practice D 1729 and instrumen tally in accordance with Method D 2244. 8. Gloss 8.1 Test in accordance with Test Method D 523. 9. Print Test 9.1 Test in accordance with Test Method D 2091. 10. Hardness 10.1 Apply a film to a clean, steel panel at a thickness agreed upon by the purchaser and the seller. Test in accordance with Test Methods D 1474. 409 DU P050297590 D 3002 11. Tape Adhesion 11.1 Test for tape adhesion in accordance with Methods D 3359. 12. Resistance to Plasticizer Migration 12.1 Test in accordance with Test Method D 2199. Time and temperature may be varied as agreed between the producer and the user. 12.2 If migration from a plastic substrate into a coating is being determined, the vinyl contact pad should be omitted. 13. Resistance to Temperature-Humidity Cycling 13.1 Expose the finished panel in accordance with Test Method D 2246. 13.2 After the number of cycles agreed between the producer and the user, determine whether adhesion (Section 11) and appearance (Sections 7 and 8) have changed. 14. Resistance to Continuous 100 % Humidity 14.1 Expose the finished panel in accordance with Prac tice D 2247. 14.2 After exposure for the length of time agreed between the producer and the user, determine whether adhesion (Section 11) and appearance (Sections 7 and 8) have changed. 15. Resistance to Household Chemicals 15.1 Test in accordance with Test Method D 1308. 16. Wear Resistance 16.1 Conduct an abrasion test in accordance with T< Method D 658 or Test Methods D 968 and determine tk abrasion coefficient. , 05 17. Light Stability Test 17.1 Expose to sunlight in accordance with Recom. mended Practice G 24. Duration of test and maxinm^ acceptable change in color shall be as agreed between the producer and the user. 18. Weather Resistance lif.L Expose panels in Florida or other area agreed be. tween the producer and the user, 45" South for 12 months and determine changes in appearance (Sections 7.2 and 8.1^ and adhesion (Section 11). t = [ ir c< 19. Resistance to Chipping 19.1 Using the plastic, pretreatment, primer, and topcoat system agreed between the producer and the user, test with the gravelometer in accordance with Test Method D 3170. I a a t 20. Effect on Substrates u 20.1 Determine the physical properties of the substrate I such as hardness, tensile strength, flexibility, or surface smoothness before and after applying the coating under test ^ 1 Select the appropriate tests for the substrate from Volumes 1 08.01, 08.02, and 08.03 of the Annual Book of ASTM I Standards. " Hi 21. Precision 21-.1 The precision of this practice is described by each i ! individual method citecL '[ The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ot infringement ot such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible techrilcai committee and must be reviewed every five years and itnot revised, either raapproved or withdrawn. Yourcomments are invited either for revision ofthis standard or toradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Bace St., Philadelphia, PA 19103. '. t! \ I1 |l ii 410 DUP050297591 Designation: D 3003 -71 (Reapproved 1987) ith Test nine the Recoin, aximum reen the reed be. months tnd 8.1), topcoat .est with >3170. ubstrate surface der test /olumes ' ASTM by each Standard Test Method for Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates1 This standard is issued under the fixed designation D 3003; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. I. Scope 1.1 This method covers determination of the pressure mottling and sticking, or blocking resistance of organic coatings applied to coil-coated or factory-coated metal prior to postformed. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2, Summary of Method 2.1 The coated metal is cut into suitably sized panels. A stack of these panels is then subjected to a specified pressure and temperature for a specified time to permit any pressure mottling and sticking or blocking to develop. The heating elements of the test apparatus are turned off and, after cooling, the specimens are examined for any signs ofsticking or blocking, and mottling. The results are rated on the 0 to 10 scale and may be used in accepting or rejecting the coating according to standards established by the purchaser and the seller. 3. Description of Terms 3.1 pressure mottling--film distortion or uneven pattern giving a change of gloss and nonuniform appearance. It is usually caused by pressures within a painted coil or stacked painted sheets or other painted products. 3.2 blocking or sticking--the condition wherein coated surfaces adhere to each other. 4. Apparatus2 4.1 A suitable hydraulic or mechanical press or vise may be used. The equipment shall be capable of producing the required test pressure in pounds-force per square inch (or kilopascals) and be equipped with a suitable device for : measuring the force applied. i 1 This method is under the jurisdiction of ASTM Committee D-l on Paint and i Related Coatings and Materials and is the direct responsibility of Subcommittee D0I.53 on Factory-Precoated Strip Metai. Edition effective Dec. 22, 1971. 2 Suitable equipment includes Pasadena or Studebaker Hydraulic Presses; Gardner Laboratories Cam-activated Pressure Mottling Tester; and drill press vises modified for use with a torque wrench if agreed between purchaser and seller f (Hensley, W. L., "Pressure Mottling Test," Journal ofPaint Technology, Vol 40, : No. 517, February 1968, p. 54/1). 5. Test Specimens and Conditions 5.1 At least four, and preferably six, flat panels shall be cut from the coated stock, die age of which shall be within the limits agreed upon by the purchaser and the seller. 5.2 Panels should be at least 4 by 2.5 in. (100 by 70 mm) to provide an adequate area for assessing the results. Where the equipment does not provide adequate pressure, smaller panels may be used. The minimum recommended size is 2 by 2 in. (50 by 50 mm). 5.3 Use only flat panels. If necessary, file the edges smooth to ensure maximum contact between the surfaces. When the equipment permits, panels larger than the pressure plates may be used, thus eliminating any effect from uneven edges. With this method, the pounds-force per square inch (or kilopascals) is calculated using only the panel area within the pressure plates. 5.4 The film thickness of the coating under test shall be as specified or agreed upon by the purchaser and the seller. 5.5 The coated stock shall be tested under the conditions of pressure, temperature, and time mutually agreed upon by the purchaser and the seller. Pressures ranging from 110 to 350 psi (750 to 2400 kPa), temperatures from 110 to HOT (43 to 60C), and times of 2 to 16 h have been used. 5.6 In the absence of agreed or specified test conditions, a pressure of 110 5 psi (750 35 kPa), a temperature of 110 3F (43 1.5C), and a time of 16 h shall be used. 5.7 The total force applied is measured by a suitable gage and the pounds-force per square inch (or kilopascals) is calculated by dividing the force (pounds-force or newtons) by the area in square inches (or square millimetres) of one side of one panel. 6. Procedure 6.1 Stack the panels face to back as used in production with both face and back coatings applied. Limit the number of panels in the test to the quantity that can be heated rapidly to and maintained at the correct panel temperature throughout the test. 6.2 For presses having heating units, place the test panels in the press and bring the heating platens in contact but with light pressure. Turn on the electrical heating unit, and heat the panels to the required test temperature. When this temperature is reached, the indicating light will shut off. Apply the required pressure and maintain it for the specified time (6.4). 6.3 Where the apparatus does not have built-in heating units, preheat the mechanical press or vise. Place the panels in the press at room temperature with very light contact and heat the unit in an oven to the required temperature. Then 411 DUP0502 97592 # D 3003 TABLE 1 Classification N0TE <--intermediate grades are permissible to distinguish smal differences, N' 2--Reasonable force Is defined as that which can be exerted by the fingers only, using the fingernails as the only prying instrument. N' 3--The transfer of components of one coating onto or into another coating Is also known as offsetting or pickoff. Grade Sticking or Blocking Grade Mottling 10 Panels fall apart--no sticking. 10 No mottling immediately after separation. 8 Slight tackiness or panels pull apart easily. 8 No mottling after 24 h separation. ' ~~~ 6 Panels pull apart with effort. No flexing or prying required to aid 6 Light permanent mottling after 24 h separation. separation. 4 Panels pull apart using reasonable force. Flexing may be required 4 Heavy permanent mottling after 24 h separation. (Note 2). 2 Panels require prying apart with a spatula or similar Instrument. 2 Light pickoff or transfer of one or both coatings (Note 3). 0 Panels block together so they cannot be separated with a spatula 0 One or both coatings show heavy pickoff down to the metal or or similar instrument, without using extreme force. basecoat; or block together (Note 3). apply the proper pressure and return the unit to the oven for the specified time. 6.4 Record the time only after the specified temperature and pressure are reached. Check the temperature and pres sure at intervals during the test. 6.5 At the end of the specified time, turn off the heat and allow the panels to cool to room temperature under pressure before removal and separation. 6.6 After removal from the press, grade the panels sepa rately for both sticking or blocking and mottling in accord ance with Table 1. In assessing the results ignore effects due to sharp or uneven edges. 6.7 Maintain panels that are to be reaccessed after a recovery period at 75 5F (24 3C). 6.8 For both properties assign each coating a grade which is the arithmetic mean of all panels tested. 7. Report 7.1 Report the following data for each coating: 7.1.1 Equipment used, 7.1.2 Number of panels tested, 7.1.3 Pressure, 7.1.4 Temperature and heating process (built-in or oven), 7.1.5 Time, 7.1.6 Grade for sticking or blocking, and 7.1.7 Grade for mottling. 8. Precision 8.1 In an interlaboratory test of this method, two opera tors in each of seven laboratories tested two different coatings, subjected to two treatments (pressure, temperature, and duration) and rated them for sticking, and pressure mottling. The within-laboratory and between laboratory pooled standard deviations were found to be as follows: Rating Parameter Pooled Standard Deviations Within- Laboratory Between Laboratory S PM Average 0.42 1.10 0.38 1.06 0.40 1.08 Based on these results the following criteria should be used in judging the acceptability of results at the 95 % confidence level. 8.1.1 Repeatability--Two results, each the mean of the two sets of panels, obtained by the same operator should be considered suspect if they differ by more than 1 to 2 units. 8.1.2 Reproducibility--Two results, each the mean of two sets of panels, obtained by operators in different laboratories should be considered suspect if they differ by more than 3.7 units. The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ol any such patent rights, and the risk of Infringement of suoh rights, are entirely their own responsibility. This standard is subject to revision at any time bythe responsible technical committee and must be reviewed every five years and If not revised, eitherreapproved or withdrawn. Your comments ate invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1919 Race St., Philadelphia, PA 19103. 1. pl cW a< a, 412 DUP050297593 Designation: D 3023 - 88 Standard Practice for Determination of Resistance of Factory-Applied Coatings on Wood Products to Stains and Reagents1 This standard is issued under the fixed designation D 3023; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A numberin parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. Wior 3er&. :reat ure( sure -ory in ce te 3 S t 1, Scope [j This practice covers evaluation of clear factory-ap0lied coating systems on wood substrates. p 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2, Referenced Documents 2.1 ASTM Standards: D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)2 D333 Test Methods for Clear and Pigmented Lacquers3 D2571 Guide for Testing'Wood Furniture Lacquers3 3. Significance and Use 3.1 When used in conjunction with Methods D 333, this practice will provide a comprehensive evaluation of resist ance to stains caused by chemical reagents and household chemicals. 3.2 This practice applies only to coatings applied in sufficient quantity to form a continuous film. It is recom mended that the dry film thickness of the coating under test be reported. 3.3 Results from stain tests conducted in accordance with this practice distinguish differences between coatings. 4. Reagents 4.1 Codefor Applicability ofReagents--V = Vertical, any surface that may be vertical as on a dresser front. H = Horizontal, any surface that may be horizontal as on a table top. L = Laboratory, any surface that may be used for laboratory furniture (Section 9). 4.2 Water: 4.2.1 Tap Water, V, H, L 4.2.2 Boiling Water (test in accordance with the Boiling Water Resistance section of Guide D 2571): H, L 4.3 Alcohol: 4.3.1 Ethyl Alcohol (test in accordance with the Alcohol Resistance section of Guide D 2571); V, H, L 1 This practice is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.S5 on Factory-Applied Coatings on Preformed Products. Current edition approved Match 25, 1988. Published September 1988. Origi nally published as D 3023 - 72. Last previous edition D 3023 - 81(1987). 1 Annual Book ofASTM Standards, Vol 06.03. 3 Annual Book ofASTM Standards, Vol 06.01. 4.4 Aliphatic: 4.4.1 Mineral Spirits: L (Specification D 235, Type III) 4.4.2 Perchloroethylene: V, H, L 4.5 Ketone: 4.5.1 Methyl Ethyl Ketone: L 4.6 Acetate: 4.6.1 Amyl Acetate: H, L 4.7 Inorganic Acid: 4.7.1 Hydrochloric Acid (3 N)--Mute 258 mL of 12 N (36 %) HC1 to 1 L: L 4.8 Organic Acid: 4.8.1 Acetic Acid (3 N)--Dilute 172 mL of 99 % acetic acid to 1 L: V, H, L 4.8.2 Grape Juice (unsweetened): V, H 4.8.3 Lactic Acid (5 % solution): V, H 4.9 Bases: 4.9.1 Unscented Mild Soap (saturated solution): V, H, L 4.9.2 Potassium Tripolyphosphate (saturated solution containing 0.5 % sodium jV-methyl-V-oleyl laurate (Igepon T-73): V, H, L 4.9.3 Ammonium Hydroxide (3 % solution): L 4.9.4 Trisodium Phosphate (saturated solution): V, H, L 4.9.5 Urea (6.6 % solution): V, H, L 4.10 Disinfectant: 4.10.1 Cresols (5 % solution): V, H, L 4.11 Ink: 4.11.1 Washable Ink: V, H, L 4.11.2 Permanent Ink: V, H, L 4.11.3 Bail-Point Ink: V, H, L 4.12 Dye: 4.12.1 Coffee (test in accordance with the Coffee Stain Resistance section of Guide D 2571): V, H 4.13 Wax: 4.13.1 Wax Crayons, Red, Blue, and Yellow. V, H 4.13.2 Lipstick (test in accordance with the Cosmetic Stain section of Guide D 2571): V, H 4.14 Shoe Polish: 4.14.1 Liquid Shoe Polish, tan: V, H 4.15 Oil: 4.2 5.1 Com Oil or equivalent: V, H 4.15.2 Hair Oil: V, H 4.16 Miscellaneous: 4.16.1 Mustard: V, H 4.16.2 Tincture of Merthiolate (1+1000): V, H (see Sec tion 5) 4.16.3 Sodium Hypochlorite (6 % solution): V, H, L 4.16.4 Tincture ofIodine--Wet 50 g of potassium iodide (KI) with water, weigh into the wet KI 70 g of iodine, let stand 1 h to dissolve the iodine, and make up to 1 L with alcohol: V, H, L V a k. k 413 i. DUP050297594 D3023 4.17 Staining Solutions, unless otherwise specified, are water solutions. 5. Selection of Staining Agents for Testing Stain Resistance of Coatings 5.1 The producer and the user shall select staining agents from the reagents in Section 4. Selection of staining agents should depend on end use, such as wall, ceiling, horizontal surface, or floor. 5.2 In the absence of agreement between the producer and the user, the suggested staining reagents for each intended use are indicated in Section 4 by V, H and L. 5.3 It is not necessary that all finishes pass all tests. 6. Test Specimen 6.1 Test panels shall be of regular production finish. 6.2 If regular production finished panels are not available, the producer and the user shall agree upon the following variables: face veneer or wood surface, filler or filler stain, primer coat, topcoat, and dry film thickness for each coating material. 7. Panel Conditioning 7.1 Before testing, panels must be aged for a time and by a method agreed upon between the producer and the user. 8. Procedure 8.1 Conduct the test with panel surfaces horizontal at room temperature unless a different temperature is specified. 8.2 Place 0.5 mL of each staining agent on the finish surface and allow to stand uncovered for 18 h (or a time agreeable to the producer and the user) except for staining agents 4.3 to 4.6. On these put a 1-in. (25-mm) square of double-acid-washed quantitative filter paper. The purpose of the filter paper is to maintain a longer wet contact of volatile reagents with the surface of the finish. 8.3 After 18 h exposure, or other time period agreed to b the producer and the user, wash the surface with water, rjn2 with ethanol (1+1) and dry with a paper towel. Place a, panel in a vertical position with a diffuse tight source aJj view (Note) from a distance of 2 to 3 ft (0,6 to 0.9 Examine the surface for graying, spotting, wrinkling, discoj' oration, or other film defects and report. N' --This method of viewing panels gives the best correlation of staining damage between laboratories. However, the following inform3, tion should be noted: U) When viewing panels across the grain at a lo angle that is being varied, many more stains will appear viable than would appear visible perpendicular to the surface. These additional stains are superficial stains only. (2) When viewing with and against % grain, there appears to be an even greater number of superficial stains than would appear when viewing perpendicular to the surface or across the grain. 9. Interpretation of Results 9.1 Each product finish differs greatly in stain resistance requirements. The key, in general, is that the resistance to staining must be adequate for that finish's end use when first used in place and throughout the expected life span of the specific product 9.2 The end use choice of resistance to staining should be agreed upon between the producer and the user. 10. Precision 10.1 Agreement between laboratories by visual compar ison varied according to how samples were viewed. 10.1.1 Stains viewed perpendicular with a diffused light source at a distance of 2 to 3 ft (0.6 to 0.9 m) for graying, spotting, wrinkling, discoloration, or other film defects gave, complete agreement between laboratories. 10.1.2 The same test stains viewed both with and across the grain at a low angle resulted in many more superficial stains being evident, depending upon the eyesight and judgment of the observer. The American Society for Testing amt Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users at this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard Is subject to revision af any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your, comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feelthat your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103: foi lat lis ea be in ai h' o 414 DUP050297595 reed to afc; lUrce a 3 0.9 ,, an at -isibli ( resistance stance to vhen firsj an of the should be compr ised light ; graying, ects gave id across iperflcial ight and Designation: D 3129 - 91 Standard Guide for Testing Exterior Latex House Paints1 This standard is issued under the fixed designation D 3129; the number immediately following the designation indicates the year of origioal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. Scope "j j. This guide covers the selection and use of procedures . testing exterior latex house paints and trim paints in the laboratory and in the field. The test methods included are Led in Tables 1 and 2. All of these may not be required for paint. Selection of the test methods to be followed must 2 governed by experience and the requirements in each jdjjVidual case, together with agreement between purchaser and seller. 1.2 This guide covers the testing of a ready-mixed latex bouse or trim paint for application by brush, roller, or spray o0 exterior surfaces. 1.3 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsi bility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 * D215 Methods of Chemical Analysis of White Linseed Oil Paints3 D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts3 D358 Specification for Wood to Be Used as Panels in Weathering Tests of Coatings3 D522 Test Method for Mandrel Bend Test of Attached Organic Coatings3 D 523 Test Method for Specular Gloss2 D562 Test Method for Consistency of Paints Using the Stormer Viscometer3 D660 Test Method for Evaluating Degree of Checking of Exterior Paints3 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints3 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints3 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints3 1 This guide is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D0J.42 on Architectural Finishes. Current edition approved Oct. 15,1991. Published December 1991. Originally Published as D 3129 - 72. Last previous edition D 3129 - 85(I990)fl. 2 Annual Book ofASTM Standards; Vols 06.01, 06.02, and 06.03. 3 Annual Book ofASTM Standards, Vol 06.01. D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D1006 Practice for Conducting Exterior Exposure Tests of Paints on Wood3 D1038 Definitions of Terms Relating to Veneer and Plywood4 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems3 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products3 D1554 Definitions of Terms Relating to Wood-Base Fiber and Particle Panel Materials4 D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature3 D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials3 D 1736 Test Method for Efflorescence of Interior Wall Paints3 D2196 Test Methods for Rheological Properties of NonNewtonian Materials by Rotational (Brookfield) Viscometer3 D2243 Test Method for Freeze-Thaw Resistance of Wa ter-Borne Paints3 D2244 Test Method for Calculation of Color Differences From Instrumentally Measured Color Coordinates3 D2369 Test Method for Volatile Content of Coatings3 D2574 Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms3 D2805 Test Method for Hiding Power of Paints by Refkctometry3 D3456 Practice for Determining by Exterior Exposure Tests the Susceptibility of Paint Films to Microbiolog ical Attack3 D3719 Test Method for Quantifying Dirt Collection on Coated Exterior Panels3 D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings3 D3928 Test Method for Evaluation of Gloss or Sheen Uniformity3 D4214 Test Methods for Evaluating the Degree of Chalking of Exterior Paint Films3 D 4287 Test Method for High-Shear Viscosity Using the ICI Cone/Plate Viscometer3 D4585 Practice for Testing Water Resistance of Coatings Using Controlled Condensation3 * Annual Book ofASTM Standards, Vol 04.09. 415 DU P0502 97596 D 3129 TABLE 1 list of Test Methods by Properties TABLE 2 Alphabetical List of Test Methods i ^ Condit Test Method Section ASTM Test Method Federal Test Method Std.No. 141 Test Method Section ASTM Test Method Federj| Test Method Std. No. )4l 4.1 Prt "tul hsurdboar Sampling 5 D 3926 Liquid Paint Properties: Condition in container Coarse particles and foreign matter Density or weight per gallon Nonvolatile Fineness of dispersion pH Consistency Rheological properties of non-Newtonian liquids Freeze-thaw stability Microorganism resistance 6.1 6.2 185 6.3 D1475 6.4 2369 6.5 D 1210 6.6 E70 6.7 0562 6.8 2196 3011 6.9 2243, D4287 6.10 D 2574 Paint Application and Film Formation: Drying properties Producing films of uniform thickness Application properties Application by brush Application by spray Touch-up uniformity 7.1 7.2 7.3 7.3.1 7.3.2 7.4 1640 823 03928 4541 2141 2131 Appearance of Dry Paint Film: Color differences by visual evaluation Color differences using instrumental measurements Daylight directional reflectance Gloss 60 Hiding power 8.1 8.2 8.3 8.4 8.5 1729 D2244 E 97 D 523 0 2805, D 344 Properties of Dry Paint Film: Flexibility Moisture blister resistance Fume resistance Exterior exposure resistance Wood panel description Chalk resistance Checking resistance Crack resistance Erosion resistance Flaking resistance Mildew resistance Stain resistance i-i Efflorescence resistance Fade resistance Dirt pickup Adhesion to chalky substrates Wet adhesion 9.1 9.2 9.3 9.4 9.4.1 9.4.2 9.4.3 9.4.4 9.4.5 9.4.6 9.4.7 9.4.8 9.4.9 9.4.10 9.4.11 9.4.12 9.4.13 522 D45B5 D 1006 D 358 0659, 04214 D660 D661 D662 D772 D 3456 D 1736 D 3719 6301 6301 Analysis of Paint: Chemical analysis Volatile content Pigment analysis 10.1 10.2 0 2369 10.3 0 215 7261 Adhesion to chalky substrates Adhesion, wet Application by brush Application by spray Application properties Chalk resistance Checking resistance Chemical analysis Coarse particles and foreign matter Color differences by visual evaluation Color differences using instrumental measurements Condition in container Consistency Crack resistance Daylight directional reflectance Density or weight per gallon Dirt pickup Drying properties Efflorescence Erosion resistance Exterior exposure resistance Fade resistance Fineness of dispersion Flaking resistance Flexibility Freeze-thaw stability Fume resistance Gloss 60 Hiding power Microorganism reslstanoe Mildew resistance Moisture blister resistance Nonvolatile pH Pigment analysis Producing films of uniform thickness Rheological properties of non-Newtonian liquids Sampling Stain resistance Touch-up uniformity Wood panel description 9.4.12 9.4.13 7.3.1 7.3.2 7.3 9.4.2 9.4.3 10.1 6.2 D 4214 D 660 185 6.1 D1729 8.2 D 2244 6.2 6.3 9.4.4 8.3 6.3 9.4.11 7.1 9.4,9 9.4.5 9.4 9.4.10 6.5 9.4.6 9.1 6.9 9.3 8.4 8.5 6.10 9.4.7 9.2 6.4 6.6 10.3 7.2 D 562 D661 E97 D 1475 D3719 D1640 1736 662 D1006 D 1210 D772 D522 D 2243 D523 D 2805, D 344 2574 0 4565 2369 E70 D215 D 823 6.8 D2196,D 4287 63o T 6301 2141 2131 4541 4091 4249 3011 5 9.4.8 7.4 9.4.1 3925 03928 D358 E 105 Practice for Probability Sampling of Materials7 2.2 U.S. Federal Test Methods Standard No. 141:* 2131 Application of Sprayed Films 2141 Application of Brushed Films 3011 Condition in Container 4541 Working Properties and Appearance of Dried Film ; 0f*asr 4.1.2 : 1 $otoe w 11 nave bci 4.1.3 1 oostU co 11 betweer 4.1-4 1 tl* UiU I contain | comple 1 4.1.1 4.i.f 1 degree I 5. Sat j 1 I shoulc { 1 rwpr 1 aw 5.2 mine DH withi and' 5.: iden 1-ga tests Pra1 6. e sep car wii CO' pai tai: Mt 6301 Wet Adhesion (Tape Test) fre E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode5 E 97 Test Method for Directional Reflectance Factor 45-deg, 0-deg of Opaque Specimens by Broad-Band Filter Reflectometry6 3. Terminology 3.1 Definitions: 3.1.1 For definitions of terms used in this practice, refer to Definitions D 16, D 1038, and D 1554. ap pa th P< D 5 Annual Book ofASTM Standards, Vol 15.05. 4 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 7 Annual Book ofASTMStandards, Vol 14,02. * Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. s\ u tl ii 416 DUPO 502 97597 Federal" Test Method Std. No. Hi 6301" 6301 2141 2131 4541 4091 4249 3011 IS7 d Film refer to Section D, () D 3129 4 Conditions Affecting House Paint Topcoats 4.1 Practical requirements and performance of latex Douse paint may vary with: 4.1.1 Substrate type, such as type and quality of wood or j^rdboard, grain of wood, knots, pitch, etc., type and quality pf masonry, ratio of cement to aggregate, alkalinity, etc. 4.1.2 Substrate weathering. Weathering of wood before painting will probably adversely affect the performance. Some weathering of masonry surfaces before painting may pave beneficial effects on the performance. 4.1.3 The type, quality, and suitability of primer, under coat, conditioner, etc., used under the topcoat and the time between coats. 4.1.4 Environmental conditions such as temperature at die time of application and during drying. As these paints contain water as a thinner, surfaces do not have to be completely dry before application. However, low tempera ture during drying may cause poor film formation. 4.1.5 Contaminants on the surface of the substrates. 4.1.6 Condition of previously painted substrates such as degree of chalk, adhesion of film, dirt, mold, general condition of substrate paint. 5. Sampling 5.1 Prior to sampling, the condition of the container should be established since damage to it may cause evapora tion, skinning, or other undersirable effects in the coating. Determine the condition of the paint in accordance with 6.1 and 6.2. 5.2 Sample in accordance with Practice D 3925. Deter mine the weight per gallon in accordance with Test Method D 1475. Repeat this procedure until successive values agree within 0.1 lb (45 g) or as agreed upon between the purchaser and the seller. Samples for testing may then be taken. 5.3 Specify the amount of sample, the package sizes, and identification codes to assure a representative sample. A 1-gal (4-L) sample is usually sufficient for the recommended tests, but for guidance in selecting a sampling plan, consult Practice E 105. 6. Liquid Paint Properties 6.1 Condition in Container--Thickening, settling, and separation are undesirable and objectionable if a paint cannot be reconditioned and made suitable for application with a reasonable amount of stirring. The referenced method covers procedures for determining changes in properties of paints after storage. Determine the condition in the con tainer in accordance with Method 3011 of Federal Test Method Standard No. 141. 6.2 Coarse Particles and Foreign Matter--Paints must be : free of coarse particles to form uniform films of good appearance, a typical maximum being 1 weight % of total paint. The specified test with a No. 325 (45-p.m) sieve gives ; the percent of these particles in a paint. Determine coarse i particles and foreign matter in accordance with Test Method j D 185. i 6.3 Density or Weight per Gallon--The density as meai sured by weight in pounds per gallon or kilograms per litre is \ used to assure product uniformity from batch to batch. In the referenced method the density is expressed as the weight i in pounds of 1 U.S. gal (kg/L) of the paint at a specified temperature. Determine the density in accordance with Test Method D 1475. 6.4 Nonvolatile--The amount of nonvolatile in a coating is not necessarily an indication of performance. It is, however, useful for determining similarity of two samples. Determine nonvolatile solids in accordance with Test Method D 2369. 6.5 Fineness ofDispersion--The more finely a pigment is dispersed, the more efficiently it is being used. One method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the material down a calibrated, tapered groove in a hardened steel block with the groove varying in depth from 4 to 0 mils (100 to 0 jim) and calibrated Hegman 0-8. The point at which continuous groupings of particles or agglomerates, or both, are visible through the surface of the liquid is taken as the fineness reading. Lower readings in mils or micrometres or higher readings in Hegman units indicate better fineness of disper sion. Determine fineness of dispersion in accordance with Test Method D 1210. N' --The fast drying of latex paints makes it difficult to make accurate measurements of this type. Low-gloss paints do not generally require dispersion finer than a 1 to 2 Hegman reading. 6.6 pH--Latex paints with low (acidic) pH may corrode the container. Changes in pH during storage may indicate poor stability of a latex paint. Determine pH in accordance with Test Method E 70. 6.7 Consistency--Paints of a given type should fall within a stated consistency range for satisfactory reproduction of a specific formula. In the referenced method, consistency is defined as the load in grams required to produce a specified rate of shear. Although the consistency of most latex paints is about 150 to 300 g/100 revolutions, a much wider range is possible because ofthe wide variations in rheological proper ties of these paints. Also two paints of the same consistency may have quite different rheological properties. Determine the consistency of the product in accordance with Test Method D 562. 6.8 Rheological Properties of Non-Newtonian Liquids-- Rheological properties are related to application and leveling properties of the liquid paint. The referenced methods cover the determination of rheological properties and are particu larly suited for use with paints that display thixotropic characteristics. They actually measure viscosity under dif ferent shear rates. Determine rheological properties in accor dance with Test Methods D 2196 or D 4287, or both. 6.9 Freeze-Thaw Stability--Water-based paints may be subjected to freezing conditions during shipping and storage. Suitably stabilized paints will resist several cycles of freezing and thawing without showing deleterious changes such as coagulation, graininess, or excessive viscosity increase. Many latex paints will increase in viscosity but can still be considered satisfactory if other properties which may be affected by a higher viscosity such as leveling and brushability are satisfactory. Determine the extent of change in several properties in accordance with Test Method D 2243. 6.10 Microorganism Resistance--Bacteria in a latex paint can cause gassing, putrefactive or fermentative odors, and loss of viscosity. Determine if the paint contains living 417 DUP050297598 # D 3129" bacteria and if it is resistant to attack by bacteria in accordance with Test Method D 2574. 7. Paint Application and Film Formation 7.1 Drying Properties--Under average conditions most flat latex paints are dry-to-touch in 1 to 2 h when the water has evaporated from the film. Slow drying of the film may result in dust pickup, poor appearance and, when used on an exterior surface, rain or dew may cause a nonuniform appearance. They can usually be recoated from within a few hours to 18 h. Curing to obtain the ultimate properties may take only a few days for some latex paints, while others may require 1 to 2 weeks depending on composition. Determine drying time in accordance with Test Methods D 1640. 7.2 Producing Films of Uniform Thickness--Methods D 823 covers the preparation of coating films of uniform thickness essential in conducting tests. 7.3 Application Properties--Application properties of a paint are generally compared to a standard or described by requirements in the product specification. Determine appli cation properties in accordance with Method 4541 of U.S. Federal Standard No. 141. 7.3.1 Brush Application--For proper method of applica tion of a brushed film for test purposes refer to Method 2141 of U.S. Federal Test Method Standard No. 141. 7.3.2 Spray Application--House and trim paints are sometimes applied by spray. Determine the spray application properties in accordance with Method 2131 of U.S. Federal Test Method Standard No. 141. 7.4 Touch-Up Uniformity--After a paint has dried, areas where less material was applied sometimes become notice able, If the paint has suitable touch-up properties, additional material can be applied to these areas only, instead of. refinishing the complete wall. The color, gloss, and leveling, of the touched-up areas and the previously coated area should be uniform. Differences in these properties are often caused by short wet-edge time, poor leveling on recoat, and pigment orientation or flotation during and after application. Determine touch-up properties in accordance with Test Method D 3928. 8. Appearance of Dry Paint Film 8.1 Color Differences by Visual Comparison--Visual comparison of color is fast and often acceptable although numerical values are not obtained. The referenced method covers the spectral, photometric, and geometric characteris tics of light source, illuminating and viewing conditions, sizes of specimens, and general procedures to be used in the visual evaluation of color differences of opaque materials. Deter mine color fence in accordance with Practice D 1729. 8.2 Color Differences Using Instrumental Measure ments--The differences in color between a product and its standard can be measured by instrument. Generally, the tolerance is agreed upon by the purchaser and the seller and may also be required if a product specification is involved. Color instruments provide numerical values that can be compared to subsequent measurements. The referenced method covers the instrumental determination of small color differences, observable. in daylight illumination, between nonfluorescent, nonmetameric, opaque surfaces such as paint specimens. If metamerism is suspected, visual evalua tion (8.1) should be used to verify the results. Calculate j5 accordance with Test Method D 2244 the color difference that have been measured instrumentally. 8.3 Directional Reflectance--This property is a measure of the appearance of lightness of a coating. It is usually assigned a value in specifications for white and pastel shadJ a typical minimum reflectance being 86 % for white wall paint. In the referenced method, the direction of illuming, tion and viewing is specified so as to eliminate the effect of gloss. Determine daylight directional reflectance in accor. dance with Test Method E 97. 8.4 Gloss 60--Gloss level can affect dirt pickup and washability. Exterior latex house paints and trim paints may vary in gloss. A typical range would be from 5 to 60 units. Determine the specular gloss in accordance with Test Method D 523. 8.5 Hiding Power (Dry Opacity)--Hiding power is the measure of the ability of a paint to hide the substrate. It is, however, dependent upon uniform film thickness which is influenced by flow and leveling. Test Method D 344 is a practical test in which paint is applied with a brush, fil thickness is approximately measured, opacity is evaluated visually as compared to a standard paint, and results are affected by flow and leveling application properties of the paint. Test Method D 2805 is considered to be a more precise and accurate test that does not need a material paint standard. Paint is applied with an applicator bar to minimize the effects of flow and leveling film thickness is rigorously measured, and opacity is instrumentally evaluated. Deter mine hiding power in accordance with Test Method D 344 or D 2805, 9. Properties of Dry Paint Film 9.1 Flexibility--Elongation is a measure of flexibility of a paint film. Generally house paints will have no problem in; passing a mandrel bend test. Most latex paints can be bent over a `A-in. (6.4-mm) mandrel without affecting the film. Determine elongation in accordance with Test Method D 522. 9.2 Moisture Blister Resistance--Moisture blister resis tance is a necessary property ofa house and trim paint. It can be evaluated by an accelerated laboratory test. Determine resistance to moisture blistering in accordance with Practice D 4585. 9/3 Fume Resistance--Fume- resistance is the ability of a dry paint film to resist -discoloration in a moist hydrogensulfide atmosphere. This type of atmosphere may be present near industrial areas and can cause paint to yellow or darken in as little'time as'.overnight exposure. There are no applicable ASTM or Federal test; methods for fume resis tance, but one method used in industry is as follows: 9.3.1 Apply a sufficient number of coats of the paint to two glass plates to hide the surface completely, allow to dry for 6 h, and expose one ofthe plates in a moist atmosphere of hydrogen sulfide for 18 h. Compare the color with the unexposed plate. The exposed plate should be no darker than the unexposed one. 9.4 Exterior Exposure Resistance--In conducting exteriorexposures, refer to Practice D 1006. 9.4.1 Wood Panel Description--In establishing exposure- 418 k*,,erfn 9-4- -rest ^ 9.4.: Test fv 9-4.1 -pest h 9.4- Test h 9-4. Test h 9.4. subjec the si especi resist* 9.4. Feder of ext of St: substi run-d kinds 9.4 conta notic subse paint 9.4 have resist volut are r resist been 9> ally late> men DUP0502 97599 Iifcfuelraetne`icem$. measure S usually el shades Kite waii Alumina! ; effect of in accor, kup arm nuts may 60 units rith Test er is the ate. It Js> which is 344 is a ush, fiim evaluated :sults are es of the a more rial paint minimize igorously i. Deter)d D 344 nlity of a oblem in i be bent the film. Method :r resist. It can termine Practice ility of a lydrogen e present >r darken are no ne resiss: paint to w to dry sphere of with the rker than ; exterior exposure ^finance, use the panels described in Specification a 4.2 Decree of Chalking--Determine the rating using Jjj Methods D 4214. `a4.3 Degree of Checking- -Determine the rating using | Method D 660. 9.4.4 Degree of Cracking--Determine the rating using re5t Method D 661. 94,5 Erosion Resistance--Determine the rating using TeSt Method D 662. 9 4.6 Flaking Resistance--Determine the rating using rat Method D 772. 9 4.7 Mildew Resistance--All exterior latex paints are -abject to microbiological discoloration that will occur on (ju surface of the coating over a period of tithe. This is jspecially true in warm, moist climates. Determine mildew jjsistance using Practice D 3456. 94.8 Stain Resistance--There is neither an ASTM' nor a federal test method available for evaluating stain resistance 0f exterior latex paints. There are, of course, different kinds 0f stain such as the water-soluble extractives in w6od substrates, the formation of lead or mercury sulfides, and top-down from metal surfaces of oxides that stain. Different lands of test methods are required for the various stains. 9.4.9 Efflorescence Resistance--Exterior latex paints can contain sufficient solid water-soluble material to cause a noticeable deposit on the film through leaching by water and subsequent evaporation. Determine the tendency of the paint to effloresce in accordance with Test Method D 1736. 9.4.10 Fade Resistance--Exterior latex paints usually bsve good color retention because of their good chalk resistance. However, the use of improper latex, pigment volume concentration, or pigments can lead to fading. There are no applicable ASTM or Federal test methods for fade 1 resistance. One method on the evaluation of chalk-fade has been published in the literature.9 9.4. L1 Dirt Pickup--Low-gloss exterior latex paints gener ally have good resistance to dirt pickup. Gloss hr semigloss latex paints may be more subject to this type of disfigure ment. Exterior exposure particularly under an .overhang wiD 5 Daiger, W. H., and Madson, W. H., "Chalk-Fade Evaluation of Tigmented Finishes by Use of Instrumentation and Computer Analysis," Journal of Paint Technology, Voi 39. No. 510,1967, p. 399. indicate a paint's tendency for this property in a relatively short time (about 1 year). Determine degree of dirt collection in accordance with Test Method D 3719. 9.4.12 Adhesion to Chalky Surfaces--Latex paints gener ally have little ability to penetrate porous substrates. There fore they do not adhere well to chalky substrates unless they are modified with some liquid that does penetrate and can bind a layer of chalk. (However certain latices do exist that are designed to adhere well to chalky surfaces. These could be considered without the need for a modifying liquid.) There are no directly applicable ASTM or Federal test methods for adhesion to chalky substrates. The industry generally uses a pressure-sensitive tape for testing this prop erty. The tape is pressed firmly onto the dried latex film (fresh dry films do not adhere as well as aged dry films) and then removed rapidly by pulling back upon itself. Method 6301 of U.S. Federal Test Method Standard No. 141 describes a similar method but includes water exposure. 9.4.13. Wet Adhesion--Determine the wet adhesion of exterior latex paints in accordance with Method 6301 of U.S. Federal Standard Test Method No. 141. 10. Analysis of Paint 10.1 Chemical Analysis--If a specification requires cer tain raw materials or certain components in a given amount, then chemical analysis is required to determine whether the specified materials are present, and in what amounts. Anal ysis does not necessarily establish paint quality that can be also greatly affected by manufacturing techniques. Most ASTM analytical methods apply to solvent-reducible coat ings. However, some of these ( 9 be adapted for analysis of water-reducible paints. 10.2 Volatile Content--The percent of volatile matter indicates the thinner loss from the film as it dries. This quantity subtracted from 100 % gives the nonvolatile con tent Determine the volatile content in accordance with Test Method D 2369. 10.3 Pigment Analysis--The analysis of pigment may be required ifthe product is covered by a specification, or if it is agreed between the purchaser and the seller. Analyze the pigment in accordance with selected test procedures from Methods D 215. 11. Keywords 1 1.1 Exterior paints; house paints; latex paints The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this, standard are expressly advised that determination of the validity of any sueft patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised', either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 419*- DUP050297600 Designation: D 3133 - 72 (Reapproved 1989)1 Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Lacquers by Infrared Spectrophotometry1 This standard is issued under the fixed designation D 3133; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. 61 N' --Editorial changes were made throughout in March 1989. 1. Scope 1.1 This test method covers the quantitative determina tion of the content of cellulose nitrate (also known as nitrocellulose) in lacquers containing alkyd resins. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Note 1. 2. Referenced Documents 2.1 ASTM Standards: D1644 Test Methods for Nonvolatile Content of Varnishes2 D 2372 Method of Separation of Vehicle from Solvent- Reducible Paints2 E 168 Practices for General Techniques of Infrared Quan titative Analysis3 E 275 Practice for Describing and Measuring Performance of Ultraviolet, Visible, and Near Infrared Spectro photometers3 3. Summary of Test Method 3.1 The method of standard additions is employed. Incre ments of cellulose nitrate, in solution, are added to aliquots of the sample. Absorbance measurements are made of the band at 848 cm-1 (11.8 pm) for each addition. The original content is then calculated from absorbance versus concentra tion. 4. Significance and Use 4.1 Coating compositions based on a mixture of synthetic resins and cellulose nitrate dissolved in organic solvents are quantitatively analyzed for the cellulosic derivative without isolating it. The test method is applicable to lacquers for which the grade of nitrocellulose is known and available. Other cellulosics, alkyd resins, many vinyl resins, and solvents do not interfere. Components, such as acrylic resins and some vinyl polymers, that absorb infrared near 848 cm-1 (11.8 pm) interfere with the determination. High boiling ester solvents, in particular methyl cellosolve acetate, may also interfere with the determination if not removed in the evaporation procedure (see 8.3). 5. Apparatus 5.1 Infrared Spectrophotometer, automatic recording, double-beam. Most infrared spectrophotometers operate from 4000 to 650 cm-1 (2.5 to 15 pm), but in this test method only the range between 1000 and 750 cm-1 (10 to 14 pm) is used. See Practices E 168. 5.2 Absorption Cells, sealed, with sodium chloride (NaG) windows, 0.1-mm path length, one pair approximately matched. 5.3 Film Vacuum Evaporator, rotary thin or equivalent apparatus, to obtain redissolvable lacquer solids without decomposition of the cellulose nitrate. 5.4 Oven, vacuum drying, thermostatically controlled to operate at 65 + 2 C. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening >the accuracy of the determination. 6.2 Cellulose Nitrate, of the same grade as in the sample. 6.3 N,N-Dimethylacetamide (DMA), spectrograde qual ity/ 6.4 Nitrogen. Gas, dry. 7. Standard Solution, 7:1 Thoroughly dry a quantity of cellulose nitrate at 65C, in the vacuum oven (Note 1). Transfer 4000 g, weighed to 0.1 mg, to a 200-mL volumetric flask. Add DMA, shake to dissolve the cellulose nitrate, and dilute to volume with DMA. One millilitre of solution is equivalent to 20 mg of 1 This method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Oct. 27, 1972. Published January 1973. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annua! Book ofASTM Standards, Vol 14.01. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagents not iislobby the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY., and the "United States Pharmacopeia." 420 cellulose N' l: dandling ai djo more tl g. proced 8.1 If quantitati proceed v 8.2 De quer, on p 1644. 8.3 Tre unpigmer the flask t of the sol in DMA, methyl cc must be t; possible. 8.4 Pip three 25-r and 10.0 < DMA. 8.5 Inf 8.5.1 S spectrome (refer to i ment). Tc and high E 275. 8.5.2 P beam. Pla solutions ( between 1 each solut nitrogen g N ' 2glass syrinf used. 8.5.3 h o.i FIG. DUP0502 97601 ar 848 High icetate, jved in ording, operate lis test 0 to 14 (NaCl) mately valent ithout lied to :hall be tended of the "hemOther at the ithout mple. , cual- 165 C, 'Jhed to take to e with mg of gents not mdards," "United D 3133 ^Uulose nitrate. VcffE 1: Warning--Every precaution must be exercised in the ndliog and drying of cellulose nitrate because of its explosive nature, than 15 g should be dried at any one time. g procedure g j If the material is pigmented, remove the pigment Quantitatively in accordance with Method D2372, and proceed with the determination on the vehicle. p g.2 Determine the nonvolatile content of the clear lacuuer, on the vehicle, in accordance with Test Methods D1644. g.3 Transfer, by any convenient means, 10.000 g of 0npigmented material to a 50-mL volumetric flask. Attach the flask to the rotary evaporator and evaporate off the bulk 0f the solvents. Detach the flask, dissolve the lacquer solids in DMA, and dilute to volume with DMA. If the presence of methyl cellosolve acetate is suspected in the solvents, care must be taken to evaporate off the solvents as completely as possible. 8.4 Pipet 10.0 mL aliquots of this solution into each- of three 25-mL volumetric flasks. To each, in turn, add 0, 5.0, gnd 10.0 mL of the standard solution. Dilute to volume with DMA. 8.5 Infrared Analysis: 8.5.1 Schedule the operating parameters of the infrared spectrometer to attain highly accurate absorbance values (refer to the directions of the manufacturer of the instru ment). To accomplish this, set for lengthier scanning time and high signal-to-noise ratio, in accordance with Practice E275. 8.5.2 Place one cell, containing DMA, in the reference beam. Place the other cell, filled in turn, with each of the solutions (Note 2), in the sample beam. Record the spectrum between 1000 and 750 cm-1 (10 and 14 pm) three times for each solution. Rinse the cell with DMA, and purge with dry nitrogen gas after each solution has been examined. No t e 2--To facilitate the transfer of the solutions to the cell, a small glass syringe fitted with a 3-in. (75-mm) hypodermic needle may be used. 8.5.3 Measure the difference in absorbance, AA, between Concentration {additions in g/25 ml) FIG. 1 Plot of AA verses Cellulose Nitrate Additions the maximum absorbance at 848 cm-1 (11.8 pm) and the minimum at 813 cm-1 (12.3 pm). Determine the mean AA for the three runs on each solution. 9. Calculation 9.1 Plot the absorbance difference, A>4, versus the cellu lose nitrate additions and extrapolate the curve to zero absorbance. The intersection of the curve with the abscissa (concentration axis) gives the original cellulose nitrate con tent in the diluted sample. See Fig. 1. 9.2 Alternative Method--Solve for C in the three simulta neous equations derived from the expression for the BeerBourguer law, A = abc A/lo/( C + 0.0) = AAoa/{ C + 0.1) = AA01/( C + 0.2) where: C = original concentration of cellulose nitrate, in grams per 25 mL and the subscripts for AA correspond to the amounts of cellulose nitrate added in grams per 25 mL. Calculate the mean of C. 9.3 Calculate the weight percent of cellulose nitrate E in the original lacquer as follows: E = {CxDx 100)fS where: D = dilution factor, S - weight of specimen, and C = grams of cellulose nitrate in 25 mL. 9.4 Calculate weight percent cellulose nitrate E in nonvol atile portion of original lacquer as follows: E = (C x 5 x 100 x 100)/(S x N) where: N -- nonvolatile content (see 8.2). 10. Precision 10.1 On the basis of a study in which four laboratories analyzed two different samples for percent of cellulose nitrate relative to the total samples, T, and relative to the nonvolatile matter, NVM, the within and between labora tory standard deviations were found to be: Percent Relative to T NVM Standard Deviations Within Between 0.14 0.12 0.39 0.64 Based on these standard deviations the following criteria should be used in judging the acceptability of results at the 95 % confidence level. 10.1.1 Repeatability--Two results obtained by one oper ator on one instrument should be considered suspect if they differ by more than the following: Relative to Percent T NVM 0.48 1.34 10.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than the following: Relative to T NVM Percent . 0.71 2.51 421 r r r k k DU P0502 97602 # D 3133 The American Society lor Tasting and Materials fates no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users ot this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or tor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may.attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Rase St, Philadelphia, PA 19103. ` 1. Scop' 1.1 T identific present tions an 1.2 1 problem user of health f limitath 2. Refe 4. Snr 4.1 filterin obtain tion ot 4.2 depoly the py chrom relativ 422 DUP050297603 Designation: D 3168 - 85 (Reapproved 1990)*1 Standard Practice for Qualitative Identification of Polymers in Emulsion Paints1 This standard is issued under the fixed designation D 3168; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. ei N' --Sections 6 to 10 were renumbered and Section 11 was added editorially in May 1990. j. Scope 1.1 This practice describes a procedure for the qualitative identification in emulsion paints of most types of polymers present as major components of the paint vehicle. Limita tions are discussed in Sections 5 and 10. 1.2 This standard does not purport to address the safety goblems associated with its use. It is the responsibility ofthe pjgr of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. % Referenced Documents 2.1 ASTM Standards: D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 D1193 Specification for Reagent Water3 D2621 Test Method for Infrared Identification of Vehicle Solids from Solvent-Reducible Paints2 E 275 Practice for Describing and Measuring Performance of Ultraviolet, Visible, and Near Infrared Spectropho tometers4 i. Terminology 3.1 Definitions--For definitions of terms, refer to Defini tions D 16. 4. Summary of Practice 4.1 The vehicle is extracted from the dried paint and after filtering is cast on a salt plate. The infrared spectrum is obtained and compared with reference spectra for identifica tion of major components. 4.2 The paint is applied to a filament and pyrolyzed to depolymerize the vehicle. An internal standard is added and the pyrolyzate is separated into its components by gas-liquid chromatography. Monomers are identified by comparison of relative retention times. 5. Significance and Use 5.1 Identification of specific acrylic polymers in emulsion paints is often difficult or impossible by infrared alone. This 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Ralated Coatings and Materials and is the direct responsibility of Subcommittee 001.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Oct. 25, 1985. Published December 1985. Originally Published as D 3168 - 73. Last previous edition D 3168 - 73 (1979)fl. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Vol 14.01. is particularly true when the acrylic is present in a small amount as a comonomer with vinyl acetate, or when blended with alkyds or other ester systems. If identification of an acrylic component is required in such a system, it may often be accomplished by gas-liquid chromatographic analysis of the pyrolyzed paint film. The presence of a number of other polymers may often also be confirmed by pyrolysis since they produce characteristic and reproducible pyrograms. 5.2 The pyrograms obtained from unknown samples vary in complexity according to the sample composition. It is necessary to establish the presence or absence of as many components as possible from a study of the infrared spectra obtained in the first part of this practice. The gas-liquid chromatography results may then be used to help identify any unknown components present and to confirm identifi cations made by infrared. 6. Interferences 6.1 Dibutyl maleate and dibutyl fumarate monomers are not successfully recovered by this procedure. If their presence is suspected as comonomer in a vinyl acetate copolymer system, n-butyl alcohol should be found in the pyrolyzate. This evidence, together with the absence of butyl acrylate or butyl methacrylate monomer peaks, is an indirect indication of the presence of one or both of these monomers. 6.2 The presence of relatively low quantities of copo lymerized adds may not be successfully established by this procedure, due to some unavoidable decomposition of acrylate and methacrylate esters to acrylic or methacrylic add and the corresponding alcohols during the pyrolysis. The infrared spectrum and an acid number determination, both run on the polymer solids, may usually be relied upon to establish the presence or absence of acid groups in the polymer. 6.3 In the case where the polymer being analyzed is simple (such as a vinyl acetate-alkyl ester copolymer, or a single acrylate-methacrylate copolymer), it might be advan tageous to examine the total pyrolyzate directly by infrared (as a solution in carbon disulfide). 7. Apparatus 7.1 Spectrophotometer, recording, double-beam, infrared, with a range from at least 2.5 pm to 15 pm and a spectral resolution of at least 0.04 pm over that range. For checking the performance of the infrared spectrophotometer, see Practice E 275. 7.2 Cell Mount, demountable. 423 DUPO 502 97604 D 3168 to the dried paint film produces a milky dispersion, ft pCCU mount 7.4 Oven, gravity or forced-draft, maintained at 105 2C. 7.5 Linear Programmed Temperature Gas Chromato drying step in 9.2 was not complete and should be repeat^ No t e 1--If there is an interest in characterization of the emulsifle, system used, the water should be filtered through a fine-texture Bit paper and taken to dryness. The solids may then be examined h! Nc geem piodi degr? graph, equipped with a thermal conductivity detector. 7.6 Pyrolysis Accessory--Any suitable apparatus for achieving pyrolysis external to the chromatograph, that results in the recovery of sufficient pyrolyzate for identifica tion purposes. The apparatus described in the Annex has been found to meet these requirements. 7.7 Gas Chromatographic Column, 10 ft (3 m) in length, t/t in. (6.4 mm) in outside diameter copper tubing packed with 10 % silicone resin5 on 80 to 100-mesh acid-washed, dimethyl-dichlorosilane treated calcined diatomaceous earth.6 7.8 Steam Bath or Low-Temperature Hot Plate.' 7.9 Flask, small Dewar. 8. Reagents 8.1 Purity ofReagents--Reagent grade chemicals shall be ' used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.7 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 8.2 Purity of Water--Unless otherwise indicated, refer ence to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 8.3 Extraction Solvent Mixture--Equal volumes of odichlorobenzene, dimethylformamide, and tetrahydrofuran. 8.4 Liquid Nitrogen. 8.5 Petroleum Ether (30 to 60C boiling range) or heptane. infrared. ^ 9.4 Dry for 15 to 20 min in an oven at 105 to 2'C. Add 50 mL of petroleum ether or heptane, cover with a watchglass, and bring to a slow boil for approximately 5 min This process removes most emulsified plasticizers, oils, and other water insoluble, nonpolymeric organic materials which might also interfere with the interpretation of thj infrared spectrum. Decant off the solvent and discard. No t e 2--If there is an interest in characterizing the water-insoluble petroleum ether-soluble fraction, it should also be filtered through fine-texture paper, taken to dryness, and examined by infrared. 9.5 Add 10 mL of the extraction solvent mixture (8.3) and place on a steam bath or low-temperature hotplate for approximately 1 h. Filter, while still hot, through a finetexture filter paper. Ifthe polymer solution is viscous, it may be diluted further with extraction solvent mixture and warmed prior to filtration. Alternatively, the pigment may be removed from the polymer solution by centrifuging. Evaporate the solution on the steam bath or hotplate to a volume of 1 mL or less. 9.6 Place the concentrated polymer solution on a halide salt crystal and spread to form a uniform film. The thickness of the film should be such that when the infrared spectrum is recorded, the transmittance of the strongest band fells between 5 and 15 %. Dry the film in an oven at 105 2C for 1 h and qool in a desiccator. 9.7 Record the infrared spectrum from 2.5 to 15 gm so that a spectral resolution of 0.04 pm is maintained throughout that range. (Methods for achieving this resolu tion will vary according to the directions of the manufacturer of the instrument used.) Addi' just F iiaay satriF 1( the supl 1C in 2 min mat N poiy; syste to O' poly prod I' coo nitr cap 1- equ 1 grai foil' 9. Procedure--Infrared Analysis 9.8 Compare the spectrum obtained with reference spectra prepared in a similar manner from emulsion paints 9.1 Transfer 1 to 2 g of emulsion paint to a 100-mL of known composition or with published collections of borosilicate glass beaker. Add approximately 2 mL of water polymer spectra such as Test Method D 2621. Other sources and swirl or use a clean glass rod to spread the paint are listed in the references (1 to 7).8 uniformly over the bottom of the beaker. 'S,! 'l.f. 9.2 Place the beaker in an oven at 105 to 2C for at least 10. Procedure--Pyrolysis-Gas Liquid Chromatography 2 h, breaking up any skins that form so that complete drying 10.1 Coat the resistance wire filament of the pyrolysis unit is ensured. 9.3 Add 50 mL of water, cover with a watchglass, and by dipping it into the original paint sample to be tested. Remove the volatiles either by drying the filament in an oven- place on a steam bath or low-temperature hotplate for 1 h. for about 30 min at 105 2C or by heating it electrically en grt of vat inti This process removes emulsifiers, protective colloids, and with the power supply set at 1 or 2 A (100 to 200C) for other water-soluble components that might interfere with approximately 10 min. If a larger volume of pyrolyzate is interpretation of the infrared spectrum. Decant off the clear required than would be produced by the initial amount of water layer and discard. If the addition of the distilled water sample deposited, additional layers of coating may be added by repeating the dipping and drying steps. 'Silicone resin SE-30 produced by General Electric Co., has been found satisfactory for this purpose. 6 Chromosorb W, manufactured by Manville Sales Corp., Filtration and Minerals, P.O. Box 5108, Denver, CO 80217-5108, has been found satisfactory for 10.2 Place the coated filament-vial cap assembly in a small beaker. Extract with water, followed by petroleum ether or heptane, as outlined in 9.3 and 9.4. 10.3 Add a few drops of liquid nitrogen to the vial or flush this purpose. 7 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem with nitrogen gas to prevent oxidation reactions from ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., tnc., New York, NY, and the "United States Pharmacopeia." 8 The boldface numbers in parentheses refer to the list of references at the end of this practice. 424 DUP050297605 on, the seated, mulsifler ure filter nined by 'C. Add with a ; 5 min. ils, and iterials, of the i. nsoluble through 3) and ate for a fineit may e and nay be Evapo'olume halide ckness rum is i falls 2C pm so tained 'esoluicturer ;rence paints ns of urces mnit 3sted. i oven rically 3) for :ate is mt of added in a )leum flush from D 3168 occurring during the pyrolysis. N' 3--If the infrared spectrum obtained in 9.8 shows poly(vinyI acetate) or poly(vinyl chloride) to be present, the pyrolysis step should be modified to prevent the acetic or hydrochloric acid formed from grading other monomers that may be present in the pyrolyzate. Addition of a drop of concentrated ammonium hydroxide to the vial just prior to pyrolysis, neutralizes the acid as it is formed. The pyrolyzate then be recovered by dissolving in diethyl ether just before sampling. 10.4 Tightly screw the coated filament-cap assembly onto the glass vial and connect the filament leads to the power supply10.5 Submerge the entire vial m liquid nitrogen contained in a small Dewar flask. Allow to equilibrate for several ojinutes, then apply a predetermined current for approxi mately 10 to 15 min. N' 4--The optimum temperature which varies for different polymer types may be determined experimentally from known polymer systems. Six amperes (approximately 600C) has been found to be close to optimum for the types tested. A study of the pyrolysis of acrylic polymers showed that heating times varying from 10 to 30 min produced no significant differences in the composition ofthe pyrolyzate. 10.6 Turn off the power supply and allow the filament to cool for several minutes. Remove the vial from the liquid nitrogen and substitute a standard screw cap for the filament- cap. 10.7 Using a syringe, add n-butyl acetate to the pyrolyzate equal to approximately 20% of the pyrolyzate volume. 10.8 Install the silicone resin column in the chromato graph and allow it to condition to 200C. Set up the following conditions on the chromatograph: Temperatures, C Injection port Detector block Column (programmed): Initial Final AT, "C/min Carrier gas: Flow rate, mL/min Detector current, mA 270 270 70 200 6 helium 60 150 10.9 Inject 5 pL of pyrolyzate into the chromatograph, engage the chart drive, and start the temperature pro grammer. Attenuate as necessary during the run. N' 5--The use of the method described minimizes the tendency of pyrolysis products to undergo secondary reactions while still in the vapor state. This simplifies the chromatograms obtained, making interpretation easier. TABLE 1 Relative Retention Times4 Monomer or Alcohol Relative Retention Methanol Ethanol Acrylonitrile Vinyl acetate Methyl acrylate Isobutanol n-Butanol Ethyl acrylate Methyl methacrylate Ethyl methacrylate n-Butyl acetate Isobutyl acrylate n-Butyl acrylate Styrene Hydroxyethyl acrylate Isobutyl methacrylate Butyl methacrylate Vinyl toluene 2-Hydroxyethyl methacrylate 2-Ethylhexanol 2-Ethylhexyl acrylate 2-Efhylhexyl methacrylate 0.13 0.16 0.25 0.37 0.45 0.48 0.57 0.65 0.72 0.93 1.00 1.15 1.29 1.33 1.38 1.43 1.55 1.64 1.64 1.72 2.31 2.56 4 Relative retention times listed are meant to serve as a guide for identification purposes. It should be understood, however, that the numbers listed are not absolute, and will vary somewhat from laboratory to laboratory and from instrument to instrument. For maximum accuracy in making identifications from retention time data, each analyst should prepare his own table by running the monomers of interest under the same conditions used for the analysis of the pyrolyzate. 10.10 Calculate retention times relative to the n-butyl acetate internal standard peak for each major peak obtained. Compare relative retention times obtained with known values for monomers of interest (see Table 1). 10.11 If any doubt remains concerning an identification based on the pyrogram obtained, it is recommended that the peak of interest be trapped as it is eluted from the chromato graph for subsequent positive identification by infrared spectroscopy or mass spectrometry. 10.12 Bum off any remaining organic residue by applying 8 or 9 A for a few seconds. Disconnect the filament from the power supply; then clean off any adhering pigment by gently brushing with a test tube brush while holding the filament under running water. The same filament may be reused many times. 11. Keywords 11.1 emulsion paints; gas chromatography; infrared anal ysis; paint vehicle; polymers; pyrolysis the end 425 DUP0502 97606 D 3168 ANNEX (Mandatory Information) Al. PYROLYSIS ACCESSORY Al.l Fig. Al.l shows 12.5 in. (320 mm) of 20 gage Nichrome wire wound in a helix configuration. The charac teristics of the filament have been chosen so that the current in amperes x 100 closely approximates the temperature of the filament in degrees Celsius. Two 0.6-in. (15-mm) lengths of 0.05 in. (1.3 mm) outside diameter. Number 18 stainless steel hypodermic tubing is crimped onto the filament ends and inserted through snugly fitting holes drilled through the cap of a 1-dram (15 by 45-mm) vial (see drawing for detail). The hypodermic tubing, which functions as a heat sink to prevent pyrolysis ofthe plastic cap, may be firmly fastened to the cap by means of an epoxy cement. A1.2 The tubing ends are connected by means of alligator clips to the leads of a suitable power supply. FIG. Al.l Pyrolysis Accessory REFERENCES 2. (1) Chicago Society for Paint Technology, Infrared Spectroscopy (4) Haslam, J., and Willis, H. A., Identification and Analysis of Committee, An Infrared Spectroscopy Atlas for the Coatings Plastics, D, Van Nostrand Co., Inc., New York, NY, 1965. Industry, Federation of Societies for Paint Technology, (5) Weinberger, L. A., and Kagarise, R. E., "Infrared Spectra of Philadelphia, PA, 1969. Plastics and Resins," OTS Bulletin No. PB-i 11438, U. S. Dept, of (2) Sadtler Commercial Infrared Spectra, Sadder Research Laborato Commeroe, May 1954. (6) Clark, G. L., Ed., The Encyclopedia of Spectroscopy, Reinhold flfr ries, Inc., Philadelphia, PA. Publishing Corp., New York, NY, 1960, p. 506-15. (3) Nyquist, R. A., Infrared Spectra of Plastics and Resins, 2nd Ed., (7) Hummel, D. O., "Infrared Analysis of Polymers, Resins, and Dow Chemical Co., Midland, MI, May 1961. Additives. An Atlas Vol I Plastics, Elastomers, Fibers, and Resins, Wiley Interscience, New York, NY, 1969. The American Society for Testingand Materials fates no position respecting the validity ofany patentrights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by tha responsible technical committee and must be reviewedevery five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your cainments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel thaf your comments have nof received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. wifi:" 'lit' ar m 426 DUP050297607 Designation: D 3170 - 87 {Reapproved 1991)e1 !nalysis of >65. Spectra of 5. Dept, of Reinhold rsins, and nd Resins, Standard Test Method for Chipping Resistance of Coatings1 This standard is issued under (he fixed designation D 3170; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of lastrevision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. This test method has been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1 N ' --Keywords were added editorially in March 1991. 1. Scope 1.1 This test method covers the determination of the ^stance of coatings to chipping damage by stones or other flying objects. N' ' 1--This test method is similar to SAE J-400. 1.2 This standard does not purport to address the safetyproblems, if any, associated with its use. It is the responsi bility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2,1 ASTM Standards: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, .Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied ' to a Ferrous Base2 . D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap-d plied to a Nonferrous Metal Base2 D1733 Method of Preparation of Aluminum-Alloy Panels for Testing Paint, Varnish, Lacquer, and Related Products3 D2201 Test Method for Preparation of Hot-Dipped Nonpassivated Galvanized Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 2.3 Other Documents: Test for Chip Resistance of Surface Coatings (J-400)4 New Pictorial Standards Coating Defects* ' This test method is under tfie jurisdiction of ASTM Committee D-1 on Paint Related Coatings and Materials and' is the direct responsibility of Subcom mittee DO 1.55 on Factory-Applied Coatings on Preformed Products. Current edition approved May 29, 1987. Published July 1987. Originally Published as D 3170-73. Last previous edition D 3170 - 74 (1980)". 2Annual Book offSTMStandards', Vot 05.0T. " "' 3 Discontinued, see 1980 Annual Book ofASTM Standards, Part 27. 4 Available from the Society of Automotive Engineers, 400 Commonwealth Watrendale, PA 15096. r s Available from the Federation of Societies for Coatings Technology, 492 ^nistown Rd., Blue Beil, PA 19422-2350. - <'.'Sv 3. Summary of Test Method 3.1 Standardized road gravel is projected by means of a controlled air blast at the coated specimens. Generally the test conditions are made more severe by performing the test at low ambient temperatures. The resultant chipping effect is evaluated by comparison with a set of photographic stand ards that appear in the Pictorial Standards Coating Defects, 4. Significance and Use 4.1 Chipping of coatings, particularly on the leading faces and edges ofautomobile surfaces, is considered unacceptable by owners. In formulating a coating or coating system to- meet service requirements, the resistance to chipping damage by flying objects such as gravel is one of the properties of importance since it can vary considerably as other properties, are adjusted. Since, resistance to chipping decreases at lower temperatures partly as the result of decreased flexibility, the test may be more directly related to service conditions by performing it at a low temperature., This test method is designed to produce a controlled amount of impact by the media on. the tcoated panel in order to enhance reproduc ibility.' "' ' 5. Apparatus 5.1 Gravel-Projecting Machine, constructed according to the design specifications shown in Fig. 1.6 5.2 Gravel--Water-eroded alluvial road gravel7 passing through a 5/s-in. (16-mm) space screen but retained on a %-in. (9.5-mm) space screen. Note that mesh screen is not a substitute for a space-screen. It is important to remove the small pieces of gravel before reusing the gravel. 5.3 Masking Tape, 4 in. (100 mm) wide.8 5.4 Temperature-Conditioning Equipment (alternatives): 5.4.1 A cold room or freezer of sufficient size in which the gravel-projecting machine and test specimens can be main tained at the specified temperature of testing. 5.4.2 A freezer or cooler in which the test panels can be cooled 10F (5C) below the specified test temperature. 5.5 Chipping Rating Standards--A set of photographic standards depicting size and number of chips in each 6 A suitable apparatus rneeungTliese specifications. can be" obtained from Q-Panel Co, 26200 First St,, Westlake, OH 44135. 7 Gravel meeting these specifications cab be obtained from Q-Panei Co., 26200 First St,, Westlake, OH 44)33; * .T *' 8 No. 202-2 masking tape manufactured by the 3M Co, St. Paul MN 55101, jhasheen found satisfactory for this purpose. 421. DUPO 502 97608 OUTLINE OF HOUSING ISOMETRIC COMPONENTS SCALE I = 1-0" FIG. 1 Gravel-Projecting Machine category (see 2.3). The photographs in Fig. 2 are for illustration purposes only and should not be used for evaluation(s). 6. Test Specimens 6.1 The composition, surface preparation, and size of specimens shall be agreed upon between the purchaser and the seller. Test panels of 4 by 12 in. (102 by 305 mm) are most suitable for this test. 6.2 The number, type, method of application, and aging of coatings shall be agreed upon between the purchaser and the seller. N' 2--Application, metal preparation, and film thickness mea surement methods are given in the following ASTM methods: D 609, D 823, D 1005, D 1186, D 1400, D 1733, and D 2201. 7. Procedure 7.1 Condition the specimens for a minimum of 1 h at the specified test temperature in the equipment specified in 5.4. Make certain the test specimens are separated and have free access to the conditioning environment so that optimum heat transfer occurs. 7.2 Adjust the air pressure on the gravel apparatus to 70 + 3 psi (480 20 kPa) with the air valve open. Keep the lid to the gravel chamber on the apparatus closed during this operation as a safety precaution. 7.3 After adjusting the air pressure, shut off the air valve, open the lid to the gravel chamber and collect 1 pt (550 mL) of graded gravel (approx 250 to 300 stones) in a suitable container. Collect the gravel by scraping across the screen to allow fines to fall through. % .* * < . % 7.4 Plac in the pan< the appara' N' 3-- the apparatu should be co the test begu 7.5 Auk ratus, plac Opening tl air stream 7.6 Mai the gravel i 7.7 Shu chamber, ; return to moisture 1 7.8 Cot masking t; pull off sic I * * v *; TA 10-24 Chips Dias Less than I mm. Illustrations 10 Chips __ S0-74 Chips 5B Dias 1-3 "" Illustrations 50 Chips FIG. 2 Reference Photographs (Illustration Purpose Onty) Ik 428 DU PO 502 97609 D 3170 1 h at the :d in 5.4. have free optimum s to 70 the lid to ring this air valve, 550 mL) suitable screen to 3C 100-150 Chips Dia: 3-6 ran. Illustration: 100 Chips Over 250 Chips Dia: Over 6 mm. Illustration: 250 Chips (Theoretical) FIG. 2 Reference Photographs (Contd) 7.4 Place one test specimen at the desired test temperature in the panel holder with the coated side facing the front of ihe apparatus and close the lid to the gravel chamber. N' 3--Due to space limitations, it may not be possible to operate ihe apparatus at the desired test temperature. In this event, the panels should be cooled below the desired test temperature by 10F (5'C) and ihe test begun within 10 s of removal from the cooler. 7.5 Automatic Gravel Feed, with automatic feed appa ratus, place one pt of the gravel in the vibrating hopper. Opening the air valve automatically feeds the gravel into the air stream over approximately a 10-s interval. 7.6 Manual Gravel Feed, with a manual feed, slowly pour the gravel into the funnel over approximately a 10-s interval. 7.7 Shut off the air valve, open the lid to the gravel chamber, and remove the tested panel. Allow the panel to return to room temperature and remove any condensed moisture by wiping dry with a cloth. 7.8 Cover the test panel with a 4-in. (100 mm) strip of masking tape. Press the tape down firmly by rubbing; then pull off slowly to remove any loose, chips of paint. 7.9 Determine the degree of chipping by comparison with the photographic standards. 8. Report 8.1 Report the substrate composition, type and age of coating, test temperature, and chipping rating. 9. Precision 9.1 Since the rating scale consists of a combination letter and number, no standard deviation value is obtainable from the supporting test results. It is the judgment of those familiar with this test method that the following precision statements are representative: 9.1.1 Repeatability--Results of tests within a laboratory differing by more than one letter or number unit should be considered suspect. 9.1.2 Reproducibility--Results of tests between laborato ries differing by more than two letters or number units should be considered suspect 10. Keyword 10.1 chip resistance The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapprovedor withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committeeon Standards, 1916 Race St., Philadelphia, PA 19103. 429- DUP050297610 Designation: D 3258 - 80 (Reapproved 1987Jl Standard Test Method for Porosity of Paint Films1 This standard is issued under the fixed designation D 3258; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates die year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. ``N' --Editorial changes were made throughout in May 1987. 1. Scope 1.1 This test method covers the determination of the porosity of a white or near white mineral spirits insoluble paint film to indicate the degree to which a subsequent coat will penetrate. 1.2 The texture of the film can affect cleanup that will influence the results of the test. A stain applied to a high-hiding paint will not lower the reflectance as much as the same stain applied to a low-hiding paint of equal porosity. These points must be considered in comparing different paints. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry12 3. Summary of Test Method 3.1 The test paint is applied to a nonporous surface, air dried, then measured for reflectance. A special colored penetrating medium is applied, the excess removed in a specified manner, and reflectance measured again. The difference between the two readings indicates the degree of porosity; the smaller the difference, the lower the porosity of the film and the greater its ability to resist penetration. 4. Apparatus and Materials 4.1 Film Applicator, 6 in. (150 mm) wide with a clearance of 12 mils (300 pm).3 4.2 Film Applicator, 5`A in. (140 mm) wide with a 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.42 on Architectural Finishes. Current edition approved Oct. 14, 1980. Published December 1980. Originally published as D 3258 - 73. Last previous edition D 3258 - 79. 1 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 3 Bird film applicators or their equivalent have been found satisfactory for this purpose. Available from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. clearance of 10 mils (250 pm).4 4.3 Rejlectometer, meeting the requirements of Test Method E 97. 4.4 Vacuum Drawdown Plate. 4.5 Camelhair Brush (approximately Vi in. (13 mm) wide). 4.6 Plastic Wash Bottle, containing odorless mineral spirits (about 16 oz (500 mL)). '4.7 Test Panel--Smooth nonporous panel such as sealed white, cardboard chart, or white plastic sheet. 4.8 Penetrating Medium--A composition of pigment and dark-colored dye dispersed in organic liquid vehicle.5 4.9 Filter Paper. 5. Procedure 5.1 Place the test panel on the vacuum plate and apply the paint under test with the 12-mil (30-pm) clearance drawdown blade. Remove the test panel from the vacuum plate and air dry 48 h under standard conditions of 73 + 3.5F (23 2C) and 50 5 % relative humidity. 5.2 Determine the percent reflectance of the dry film using the green filter on the reflectometer. When making this reading, back up the panel with a flat rigid opaque object and mark the area on which the reading was made. 5.3'Place the panel containing the dry paint film on the vacuum plate. Using the 10-mil (25-pm) clearance blade, apply the penetrating medium over the test paint, covering the area marked as above and drawing the applicator blade in the same direction as before. 5.4 After 5 min + 15 s wash off excess penetrating mcdium.To do this, hold the panel vertically and remove the medium using the camelhaii brush wet with odorless mineral spirits. Repeat the process until most of the excess is removed. Then continue to remove more of the excess by applying mineral spirits directly from the wash bottle to the area above the stain so that it Bows across the stained area. Pause to observe the bead that forms at the bottom of the panel. If the bead is not clear, continue washing with mineral spirits until the bead is essentially clear. Test with filter paper to be sure no dye remains in the bead. 5.5 Hang the panel in a vertical position and air dry for 3 h. As before, read the percent reflectance over the same area A The Dow latex film caster has been found satisfactory for this purposeAvailable from BYK*Gardner, Inc., Gardner Laboratory, 2435 Linden Silver Spring, MD 20910. 5 Available from: K & N Laboratories, Inc., 5331 Dansher Rd., Countryside, & 60525. I jtg&gsmsasstts 430 ofthe pi panel. 6. Repo 6.1 R of the ui 7. Preci 7.1 O method tested p porosity, standard Nomina in Refl DUP05029761 1 of Test (13 mm) mineral as sealed ment and e.5 D 3258 fthe pa1161 with the same flat rigid opaque object behind the nel. t Report g 1 Report the difference between the percent reflectance untested film and that of the penetrated film. j precision *71 On the basis of an interlaboratory study of this test tjiod in which one operator in each of ten laboratories ted paint films of two nominally different levels of ' tosity, the within-laboratory and between-laboratories ^ndard deviations were found to be: Nominal Difference in Reflectance, % 7 35 Standard Deviations Within-Laboratory Between-Laboratories 0.27 1.26 0.60 4.22 Based on these standard deviations the following criteria should be used to judge the precision or results at the 95 % confidence level: 7.1.1 Repeatability--Duplicate results, obtained by a single operator, should be considered suspect if they differ by more than 0.8 % relative for difference in reflectance levels of about 7 % and more than 1.8 % relative for difference in reflectance levels of about 35 %. 7.1.2 Reproducibility--Two results, each the mean of duplicate measurements obtained in different laboratories should be considered suspect if they differ by more than 4.0 % relative for difference in reflectance levels of about 7 % and 14 % relative for difference in reflectance levels of about 35%. 8. Index Terms 8.1 This test method is indexed under the following terms: porosity; resistance--penetration (into paint films). The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and It not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. apply the clearance : vacuum of 73 + dry film iking this bject and m on the ~e blade, covering or blade tetrating love the mineral excess is ixcess by tie to the ned area, m of the i mineral ter paper dry for 3 ame area iiis purpose, mden Lane, tntrysi.de, IL 431 DUP05 0297612 dhIB Designation: D 3259 - 84 (Reapproved 1990)61 Standard Practice for Infrared Determination of the Temperature of Applied Coatings on Wood Products During the Curing Cycle1 This standard is issued under the fixed designation D 3259; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. N' --Section 5 was editorially changed in May 1990. angle of respond: length re by stray 1. Scope 1.1 This practice is intended to serve as a guide in measuring with infrared instruments the temperature during, the curing process of coatings applied to wood products. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. designed with a narrow or broad band pass and may compensate for changes in ambient temperatures. One instrument3 with the latter feature has a band pass of 8 to 14 I pm. Another instrument4 that must be rezeroed to compen. sate for changes in ambient temperatures has a band pass of 3 to 20 pm. However, this instrument can be completely portable and requires essentially no warm up time. 3.3 Thermalvoltaic Type5--These instruments are equipped with collection chambers for radiated energy that then heat a thermocouple to the temperature of the surface 2. Significance and Use 2.1 The forest products finishing industry has encoun tered difficulties in measuring the temperature of painted surfaces during the curing process. The use of thermocouples is not entirely satisfactory because the thermocouple wires tend to conduct heat away too rapidly from the area where the temperature is being measured. Infrared radiation ther mometers that are simple to operate can circumvent this difficulty. After calibration they are aimed at the surface, measured. As such, they require a minimum target area off in. (25 mm) in diameter and have a delay time that averages about 1.5 s. 3.4 Instrumentation is available for on-line process monitoring control of product temperatures. These units have long term stability that permits operation in varying ambients encountered in plants or mills without periodic calibration. The instruments also have output signals to operate recorders and controllers. ; | I switched on, and the temperature read directly from an 4. Procedure indicating gage. 4.1 Calibration--Calibrate each instrument according to N' 1--Temperature-sensitive crayons, papers, and pellets may be successfully used to measure only the highest temperature reached by the instructions of the manufacturer. A standard blackbody [ capable of being controlled at various temperatures is almost ; painted surfaces during the curing cycle. essential for calibration. One such blackbody6 is a modified 2.2 There are several different types of infrared radiation hot plate with a `/2-in. (13-mm) thick aluminum plate and a thermometers, including those based on lead sulfide or ventilated cowling to minimize the effects of ambient drafts. thermistor sensors and those that are simple thermal voltaic A dial thermometer with its stem within the aluminum plate | transducers. As such they respond to different wavelengths of serves to monitor the temperature of the blackbody. j i infrared radiation and have different areas of applicability. 4.2 Operation: \ 1 Only instruments that have been evaluated are included in 4.2.1 Detailed instructions on the operation of each i this practice. instrument are not included in this practice. Unless other- wise agreed follow the manufacturer's instructions in oper- | 3. Apparatus 3.1 Lead Salt Types1 (Note 2)--Two lead salts are com monly used. Lead sulfide that responds to wavelengths between 1.0 and 3.0 pm and lead selenide that responds to wavelengths between 15 and 4.5 pm. 3.2 Thermistor Type--Thermistors are sensitive to longer ating the equipment. 4.2.2 One general precaution is that the instrument must observe only the surface being measured and not stray radiation from infrared heaters, sunlight, electric lights, or other sources. The permissible distance from the surface to the sensor depends upon the area of surface, the viewing \ wavelength infrared of 3 to 20 pm. Instruments may be 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of DO 1.52 on Factory Coated Wood Products. Current edition approved Aug. 31, 1984. Published January 1985. Originally published as D 3259 - 73. Last previous edition D 3259 - 73. 2 The Williamson 1200 manufactured by the Williamson Development Co., lncM West Concord, MA 0178 L, is an example of this type. 3Optitherm II Model 8014 manufactured by Barnes Engineering OsStamford, CO 06904, is an example of this type of instrument. 4 Raynger R2LT manufactured by ftaytek, Inc., Santa Cruz, CA 95060, is to example of this type of instrument. 5 Kustotberm B distributed by Epic Inc., New York, NY 10038, is an exampb of this type of instrument. 6 Field Calibration Source, Model 11-101 manufactured by Baines Engineeri Co., Stamford, CO 06904. ; j i: | j 432 DUP050297613 D 3259 -le of the instrument and the wavelength that the sensor ^p0nds to. Instruments operating only in the long wave- path region of the infrared spectrum are affected much less jy stray radiation and by color variations. 5. Keywords 5.1 cure temperature; infrared; paint surface temperature; temperature measurement; wood coating The American Society for Testing and Materials takas noposition respecting the validity ofanypatent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ofInfringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be'revtewed every five years and Itnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ind may res. One :>f8 to 14 compel. ld pass of >mpletely nts are ergy that e surface area ofi averages ess mon ths have varying periodic ignals to jrding to lackbody is almost modified e and a t drafts, m plate >f each other- in oper- ;nt must iot stray ights, or rrface to viewing :ering Co.. >5060, is an example Engineering j \ : : DUP050297614 Designation: D 3260 - 82 (ReapprovedT991) Standard Test Method for Acid and Mortar Resistance of Factory-Applied Clear Coatings on Extruded Aluminum Products1 This standard is issued under the fixed designation D 3260; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (f) indicates an edildrial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the evaluation of the mortar and acid resistance of clear protective coating factors applied to extended aluminum substrates. 2. Referenced Documents 2.1 ASTM Standards: C207 Specification for Hydrated Lime for Masonry Purposes12 D823 Test Method for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 3. Summary of Test Method 3.1 Panels that have been buffed, cleaned, neutralized, and coated with the material being evaluated are exposed to freshly prepared mortar and to a hydrochloric acid solution. 4. Significance and Use 4.1 This test method will provide differentiation between types of coatings for acid and motor resistance providing the coating is applied in a uniform continuous film with a specified film thickness. 5. Reagents 5.1 Acid--Ten volume percent solution of commercial grade hydrochloric acid (31.4 to 31.8% HC1, 20Be) in distilled water. 5.2 Cleaning Solution--An alkaline cleaner4 in the con centration recommended by the manufacturer, usually 6 to 8 oz/gal (45 to 60 g/L) of water. The pH of the solution should be between 11.4 and 12.2. 5.3 Lime--Building lime complying with Specification C 207. 5.4 Neutralizing Solution--Prepare from a stable freeflowing, granular material having a chromate base5 as recommended by the supplier, usually at a concentration of 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Oct. 29, 1982. Published January 1983. Originally published as D 3260 - 73. Last previous edition D 3260 - 73 (1978). 2 Annual Book ofASTM Standards} Vol 04.01. 3 Annual Book ofASTM Standardsf Vol 06.01. 4 Diversey No. 808 has been found satisfactory for this purpose. 5 Diversey No. 814 has been found satisfactory for this purpose. 12 to 16 oz/gal (90 to 120 g/L) of water. 5.5 Sand--Dry sand capable of passing through a lfl. mesh wire screen. 6. Test Panels 6.1 Panels of extruded aluminum alloy No. 6063-T5 with dimensions 6 by 3 by `A in. (150 by 75 by 6.3 mm) shall be used for the test. 7. Procedure 7.1 Preparation of Test Panels: 7.1.1 Buff the aluminum panels and remove the buffing compound with an organic solvent. 7.1.2 Immerse the panels in cleaning solution (5.2) for 1 h at a temperature of 200F (93C). 7.1.3 Rinse the panels in tap water having a pH of 6.5 to 7.5 until the surface is free of water break. Use reagent water for rinsing if the pH of the tap water is outside the specified limits. The panels shall be free from evidence of corrosion or surface attack. 7.1.4 Immerse the panels in neutralizing solution (5.4) at 75 2F (24 l'C) for 30 s to neutralize any retained alkalinity and to promote adhesion of the applied coatings. 7.1.5 Rinse the panels in reagent water and allow them to dry a minimum of 1 h before coating. 7.2 Coating of Test Panels: 7.2.1 Apply the coatings being evaluated to the test panels in a uniform continuous film by automatic spray equipment \ in accordance with Method A of Test Method D 823. 7.2.2 For the mortar test, spray two panels on one side with two or more full wet coats to produce a minimum dry | film thickness of0.6 mils (15 pm) and two panels with one or ; more full wet coats to produce a minimum dry film thickness of 0.3 mils (7.5 pm). 7.2.3 For the acid test, spray two panels with two or more full wet coats, on both sides, to produce a minimum dry film < thickness of 0.6 mils (15 pm) and two panels with one or more full wet coats on both sides to a minimum dry film thickness of 0.3 mils (7.5 pm). 7.2.4 Allow the panels to dry for 7 days at 73 3.5F (23 2C) and 50 5 % relative humidity. 7.3 Mortar Test: 7.3.1 Prepare freshly mixed mortar by dry mixing 75 g of building lime (5.3) and 225 g of sand (5.5) and adding sufficient reagent water while stirring to make a soft paste that can be formed into a firm mortar patty approximately 1 y% in. (40 mm) in diameter and lA in. (6 mm) thick. 7.3.: test pa 7 days 3.5 7.3.: cabine the pa 7.3.surfao light i Exam: disco! part b each i 7.4 7.4. 434 DUP050297615 a 10- '5 with hall be buffing for 1 h r 6.5 to t water lecified sion or !5.4) at stained itings. hem to # D 3260 7.3.2 Apply the mortar to the top and bottom areas of the test panels and, without drying, immediately expose them for 7 days at 95 to 98 % relative humidity at a temperature of 70 * 3.5F (21 2C) in an automatically controlled cabinet. 7.3.3 At the end of 7 days take the panels from the test cabinet and immediately dislodge the mortar patties from jjje panels using a damp cloth to remove any residue. 7.3.4 View the surface of the panels perpendicular to the sUrface under a diffused light source providing a minimum jjght intensity at the surface of 200 ft-candles (2150 lx). Examine for blistering, peeling, lifting, crazing, flaking, or ^coloration of the coating, and for corrosion of the coated part of the aluminum panel. Three observers shall evaluate each panel and the majority assessment shall govern. 7.4 Acid Test: 7.4.1 Apply a mixture of 50 parts beeswax and 50 parts paraffin to protect the raw edges to a distance of 3A in. (10 mm). 7.4.2 Immerse the panels, in the acid bath (5.1) at 70 3.5F (21 2C) for 6 h. Remove the panels, rinse in water, and allow to dry. 7.4.3 Examine and evaluate as in 7.3.4. 8. Precision 8.1 The effect of acid and mortar on the coatings is expressed in terms of appearance and numerical values are not generally assigned. 8.2 In a cooperative test program, consistent results were obtained by all cooperators when all of the test variables were controlled closely. The success of the procedure depends particularly on having a continuous film of the coating on the panels, the proper pH value when rinsing the panels, and proper protection of the edges of the panels in the acid test. The American Society for Testing and Materials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia. PA 19103. panels ipment e side m dry me or film ; more Iry film one or ry film 5F (23 75 g of adding ft paste imately ; . 435 D UP050297616 Designation: D 3271 - 87 Standard Practice for Direct injection of Solvent-Reducible Paints Into a Gas Chromatograph for Solvent Analysis1 2 3 should be sample bo with nom solvent or This standard is issued under the fixed designation D 3271; the number immediately following the designation indicates the year of original adoption or, in the case of revision, Ihe year of last revision, A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice describes the techniques used to inject whole paint samples directly into a gas chromatograph to obtain a chromatogram from which the solvent composition may be established.2,3 1.2 This practice is not designed to be quantitative. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine ihe applicability of regulatory limitations prior to use. A specific hazard statement is given in 6.1. 2. Referenced Document 2.1 ASTM Standard: E 260 Practice for Packed Column Gas Chromatography4 3. Summary of Practice 3.1 A suitable aliquot of whole paint is injected, by means of a syringe, into a gas chromatographic column in order to separate the solvents. 4. Significance and Use 4.1 Gas chromatographic separation of solvents present in whole paints is the preferred first step for identifying and quantitating solvent compositions, using auxiliary proce dures and techniques. 5. Apparatus 5.1 Gas Chromatograph--Any instrument with tempera ture programming capability may be used. It should be equipped with either a thermal conductivity or flame ioniza tion detector (see Practice E 260). 5.2 Recorder--A 1 to 10-mV recorder with a full-scale response time of 2 s or less and a maximum noise of 0.03 % of full scale. 5.3 Column--The resolution of the column must be such that under the operating conditions selected the distance from the base line to the depression between two adjacent peaks must be not more than 50 % of the smaller peak, Columns may be either packed or capillary. 6. Reagents and Materials 6.1 Carrier Gas--Helium or hydrogen for use with thermal conductivity detector units; and nitrogen, helium or argon for use with flame ionization detector units. N' 1: Precaution--When hydrogen is used, special precautions should be taken to prevent gas leakage from causing a possible explosion.5 6.2 Column Packing Material, meeting requirements in 5.3. The following materials have been used satisfactorily: 6.2.1 Polyethylene glycol, molecular weight 20 000,6 and diisodecyl phthalate as liquid phases on a solid support of 60 to 80 mesh (250 to 175 pm) diatomaceous earth. 6.2.2 Porous beads of ethylvinylbenzene and divinylbenzene copolymer,7 60 to 80-mesh (250 to 177-pm) have also been successfully used as column material. 6.3 Liquid Charging Devices, such as micro syringes.8 Disposable type is preferred. 6.4 Septum Sample Vials, PTFE-fluorocarbon-faced.9 7. Procedure 7.1 Protect the injection port from the nonvolatile portion of the paint by using a borosilicate glass injection port sleeve (Note 2), glass wool plug, or by any other suitable means, If the whole paint sample is of sufficiently low viscosity, draw an aliquot directly into the syringe. When the whole paint sample is too viscous, dilute with a suitable solvent (Note 3) that will not interfere with the analysis. In order to minimize solvent losses due to evaporation, the whole paint sample 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved June 26, 1987. Published August 1987. Originany published as D 3271 - 73 T. Last previous edition D 3271 - 76(1981)el, 2 New York Society for Paint Technology, Technical Committee 76, "The Application of Gas Chromatography to the Analysis of Coating Solvents," Journal ofPaint Technology, Vol 40, No, 516, January 1968, pp. 33-48. 3 Esposito, G. 0,, aud Swann, M. H., "Direct Analysis of Solvents in Lacquer by Programmed Temperature Gas Chromatography," Official Digest Federation Society Paint Technology, Vol 33, No. 440, September 1961, pp. 1122-1131. 4 Annual Book ofASTM Standards, Vol 14.01. 5 Consult Pamphlet G-5, available from the Compressed Gas Association, lac., 500 5th Ave., New York, NY 10036. 6 Carbowax 20M, available from Union Carbide Corp., 270 Park Ave., New York, NY 10017, has been found suitable for this purpose. 7 Porapak Q, available from Waters Associates, lac., 34 Maple St, Milford, MA 01757, has been found suitable for this purpose. 8 Disposable syringes, available from Precision Sampling Corp, P.O. Box 15886, Baton Rouge, LA 70895, have been found suitable for this purpose. 5 Vials, available from Pierce Chemical Co., P.O. Box 117, Rockford, DL 61105, have been found suitable for this purpose. I j ; i 436 DUP050297617 full-scale noise of st be such distance 1 adjacent Her peak. D 3271 ,ollld be placed in a PTFE-fluorocarbon-faced septum ^0ple bottle prior to being drawn into the syringe. Proceed vjtk normal techniques to obtain a chromatogram of the jvent or solvents present in the sample. N' 2--Consult manufacturer of particular instrument used. N' 3--Ethyl ether and methylene chloride have been found satisfactory for most sample types. The American Society for Testing and Materials takes no position respecting the validity of any patera rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is sub/ect to revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised, eitherreapprcwed orwithdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Race St., Philadelphia, PA 19103. use with helium or precautions a possible :ments in ictorily: 000,6 and port of 60 vinylbenhave also syringes.8 aced.9 portion rt sleeve leans. If ty, draw >le paint . (Note 3) minimize it sample jciation, Inc., k Ave., New Milford, MA P.O. Bos urpose, >rd,IL 61105. 437 DU PO 502 97618 Designation: D 3272 - 76 (Reapproved 1988)e1 Standard Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis1 This standard is issued under the fixed designation D 3272; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies of the Department of Defense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1 N !' --Editorial changes were made throughout, including the title, in February 1988. \ 1. Scope 4.4 Safety Shield. | 1.1 This practice covers a vacuum distillation procedure that separates the solvents from the nonvolatile portion of paints so they may be analyzed. 1.2 An alternative procedure for the analysis of solvents in paints is described in Practice D 3271. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1. Referenced Document 2.1 ASTM Standard: D 3271 Practice for Direct Injection of Solvent-Reducible Paints into a Gas Chromatograph for Solvent Analysis2 3 3. Summary of Practice 3.1 The sample of whole paint with added tricresyl phosphate is heated by means of a silicone oil bath. The distillation is allowed to proceed for a period of time and then vacuum is applied. Finally dry air is passed through the system to facilitate the removal of any high-boiling solvents present. 5. Reagents ' 5.1 Methylene Chloride or Acetone. 5.2 Silicone Oil.5 5.3 Tricresyl Phosphate. \ 6. Procedure 6.1 Immerse the receiver in a bath containing dry ice with methylene chloride or acetone of sufficient depth that the liquid reaches to the bottom level of the rubber stopper. 6.2 Pour approximately 15 g of the whole paint sample into the 50-mL distillation flask. Immediately follow with 10 mL of tricresyl phosphate and without delay mix the contents of the flask. 6.3 Assemble the apparatus and close the needle valve and stopcock attached to the capillary tubing. Immerse the distillation flask by raising a silicone oil bath preheated to 155 to 160C (Warning--see Note 1) until it reaches the side arm (Note 2). Allow the distillation to proceed for 15 min without vacuum. j ! \ f I s No t e l: Warning--Care should be taken to prevent the temperature of the silicone oil exceeding 160'C because of possible formation of explosive mixtures of air and solvents from the sample being analyzed. No t e 2--The liquid level in the oil bath should be as high, as is practical. | i ? 4. Apparatus 4.1 Apparatus5 is shown in Fig. 1. It is essential in assembling this apparatus, that the volume of the portion preceding the flask be kept to a minimum by using diameters of connections and distances as small as possible. Include a gage in the assembly for measuring pressure. 4.2 Vacuum Pump, capable of pulling 2 mm Hg or less of vacuum pressure. 4.3 Septum Sample Vial, PTFE-fluorocarbon-faced.4 1 This practice is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.21 on Chemical Analysis of Paints and Paint Material. Current edition approved Oct. 29, 1976. Published December 1976. Originally published as D 3272 - 73 T. Last previous edition D 3272 - 73 T. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Obtainable from SGA Scientific, Inc., 735 Broad St., Bloomfield, NJ 07005. 4 Septum vials available from Precision Sampling Corp., Baton Rouge, LA 70315, have been found satisfactory for this purpose. 6.4 After 15 min apply vacuum slowly and carefully to \ avoid bumping or rapid distillation until 2 mm Hg is | reached. This step should take approximately 10 to 15 min, j Next, carefully open the stopcock. After bubbling subsides, | adjust the needle valve so as to regulate the flow of air at a i rate of 60 to 80 bubbles per minute (at the bubble counter). | Pass air through the system for a total of 30 min while ; f keeping the dry ice bath at a minimum low temperature. \ 6.5 At the end of the 30-min period release the vacuum f very slowly with air flowing to prevent back-up of the paint. | Remove the receiver containing the solvents and warm the | j contents only to the temperature of cold running tap water. | Transfer the isolated solvents promptly to an airtight septum | faced vial for subsequent analysis. I 5 Silicone oil 710 available from Dow Coming Corp., Midland, MI has been | found satisfactory for this purpose. | -31$ m438- DUP050297619 Heedle voivtf D 3272 ce with hat the jer. sample Mth 10 tix the Ive and 'se the ated to he side 15 min nerature tion of alyzed. h as is illy to Hg is 5 min. bsides, ur at a unter). i while ure. acuum : paint, rm the water, leptum FIG. 1 Distillation Apparatus The American Society lor Testing end Materials takes no position respecting the validity ofany patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Race St., Philadelphia, PA 19103. 439 DU PO50297620 i Designation: D 3273 - 86 (Reapproved 1991)61 Standard Test Method for Resistance to Growth of Mold on the Surface of Interior Coatings in an Environmental Chamber1 This standard is issued under the fixed designation D 3273; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense S1 N"#' --Keywords were added editorially in July 1991. f. 1. Scope 4. Apparatus 1.1 This test method describes a small environmental 4.1 Environmental Chamber, capable of maintaining a f chamber and the conditions of operation to evaluate relative humidity of 95 to 98 % at a temperature of 90 2T j reproducibly in a 4-week period the resistance of a paint film to surface mold growth in a severe interior mold environ-' ment. The apparatus is designed so it can be easily built or (32.5 1 C) while providing a continuous'inoculation oftie | surface of exposed panels with mold spores. The chamber f should be kept in a room controlled to 70 to 75F (21 to I obtained by any interested party and will duplicate results 24t"C) so that heat loss from the cabinet is insignificant and f obtained in a large tropical chamber. that 95 to 98 % relative humidity is readily obtained at the J 1.2 Temperature and humidity must be effectively con test temperature. Alternatively the cabinet must be insulated j trolled within the relatively narrow limits specified in order with suitable materials to minimize heat loss. | for the chamber to function reproducibly during the short test period. Severity and rate of mold growth on a film is a 4.2 Small Cabinet, suitable for holding about twenty-five ' 3 by 4-in. (75 by LOO-mm) test panels under these conditions j if function of the moisture content of both the film and the can be constructed as follows (Fig. 1): ? substrate. A relative humidity of 95 to 98 % at a temperature 4.2.1 Tank, polypropylene or polyethylene, with an offset \ i of 90 2F {32.5 TC) is necessary for test panels to shoulder at the top rim is used as the chamber.3 A pitched ! develop rapidly and maintain an adequate moisture level to top with straight sides should be Constructed out of acrylic } support mold growth. plastic so moisture condensation will run down the sides and : 1.3 This standard does not purport to address all of the be recirculated instead of dripping onto the panels. safety problems, if any, associated with its use. It is the 4.2.2 Heating Coil,4 125-W, regulated by a controller5 [ responsibility of the user of this standard to establish appro and installed in the bottom of the chamber by connections priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. through the end wall. It is so placed that it is immersed when ; there are 2 to 3 in. (50 to 75 mm) of water in the bottom of j dicu tray 2. Referenced Document the chamber. A 90F (32.5C) thermostat should be installed : spo in the chamber in the area by the test panels to regulate the j the 2.1 ASTM Standard: heat input through the controller to the heating coil in the : 4. D3274 Test Method for Evaluating Degree of Surface water. j the Disfigurement of Paint Films by Microbial (Fungal or Algal) Growth or Soil and Dirt Accumulation2 4.2.3 Tray, stainless steel or plastic, approximately 1 in. j test (25 mm) smaller than the inside dimensions of the chamber ! appi & 3. Significance and Use H and 1 to 3 in. (25 to 75 mm) deep with a noncorrodible ` soil metal6 mesh bottom should be supported 1 in. (25 mm) : with 3.1 An accelerated test for determining the resistance of above the water level and centered in the chamber. One layer used interior coatings to mold growth is useful in estimating the of fine plastic or fiberglass screen should be placed over the may performance of coatings designed for use in interior environ metal mesh for holding soil. ments that promote mold growth and in evaluating com 4.2.4 Small Fan,1 mounted through the end wall perpen- Nc pounds that may inhibit such growth and the aggregate levels rate a for their use. 4.1 i 3.2 This test method should preferably be used by persons who have had basic microbiological training. } Dynalab Coip., Rochester, NY, and Cole Parmer Instrument Co., Chicago, R have tanks of this type available in dimensions approximating 27 by J 8 and 18 in. (686 by 457 and 457 mm) high. ' test ' 4 The Chromalox* heating coil manufactured by the Wiegand Div., Emerson 5. R Electric Co., Pittsburgh, PA has been found satisfactory for this purpose. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint 5 The Lumenite Electronic Level Control has been found satisfactory for this 5.1 and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.28 on Biodeterioration. Current edition approved May 30, 1986. Published July 1986. Originally published as D 3273 - 73 T. Last previous edition D 3273 - 82*L 2 Annual Book ofASTM Standards, Vol 06.01. purpose. 6 Monel has been found satisfactory for this purpose. 1 i/250-hp fan operating at 300 r/min with a 1.5-in. blade, obtained fro Dayton Electric Manufacturing Co., or equivalent, has been found satisfactory for this purpose. suita pHo becoi 5.2 440 DUP050297621 aining a 90 2'F on of the chamber F (21 to cant and cd at the insulated enty-five mditions an offset . pitched )f acrylic sides and introller5 inections led when ottom of 'nstailed late the 1 in the ly 1 in. hamber rrodible 25 mm) One layer over the 1 perpen- Chicago, 1L 8 and 18 in. v,, Emerson >se. lory for this tained from isfactory for # D 3273 5.2.1 Aureobasidium pulluians} ATCC 9348 5.2.2 Aspergillus nigerf ATCC 6275 5.2.3 Penicilliumf Sp. 12667 or ATCC 9849 5.3 Test Panels: 5.3.1 Ponderosa Pine (Pinus ponderosa Laws) Sapwood Panels, Vi in. (12.7 mm) thick, 3 by 4 in. (75 by 100 mm), free of excessive resins, knots, growth rings or other abnor malities, surfaced smooth on four sides. Wood shall be kiln dried after sawing to avoid infestation of wood-rotting fungi and any wood showing evidence of such infestation shall be eliminated as test material. Wood shall be weighed after conditioning at room temperature in a dry room to 15 % moisture content. Calculated weight shall fall between 6.0 and 7.0 g/in.3 (365 and 425 kg/m3). Panels containing heartwood areas should not be used as they will inhibit mold growth under test conditions. 5.3.2 Gypsum Board Panels, lh in. (12.7 mm) thick, 3 by 4 in. (75 by 100 mm). N&'' 2--Other substrates may be used but may result in a different rate or severity of mold growth. dicular to and just above the surface of the soil bed in the tray (4.2.3) to provide dispersion and circulation of the mold spores to achieve continuous inoculation of the surfaces of the painted panels. 4.2.5 Series of Wood Bars, suspended across the width of the chamber at a height and spacing that allows the use of test panels 3 by 4 in. (75 by 100 mm), hung vertically, with approximately 3-in. (75-mm) clearance above the inoculated soil with a suitable method of fastening. Screw eyes are used with the wooden panels while a wire frame or a large clip is used with the gypsum board panels. Other support systems may be utilized. N$%' 1--Other angles of exposure may be used but may alter the rate and severity of mold growth. 4.3 Psychrometer, for measuring relative humidity in the test area. 5. Reagents and Materials 5.1 Soil--A good quality greenhouse-grade potting soil, suitable for plant propagation, containing 25 % peat moss. PH of the soil should fall from 5.5 to 7.6. Do not allow soil to become compacted. 5.2 Cultures: 6. Preparation of Apparatus 6.1 Place greenhouse soil in the tray in the cabinet and add water to the tank chamber to the desired depth. Allow the cabinet to equilibrate for 24 h before inoculating the soil with the specified mold suspensions. 6.2 Prepare mold slants of all three cultures and age 10 to 14 days or purchase prepared mold slants8 of all three cultures. Prepare mold suspensions from each type of mold slant by the following procedure: Add one drop of 25 % nonionic surfactant9 solution to 95 to 100 mL sterile deionized or distilled water and shake. Pipet 5 mL of this solution onto the mold slant. Scrub the surface of the slant with a sterile cotton swab to remove as much spore and mycelial growth as possible without digging up the surface of the agar. Pour the water from the scrubbed slant back into the surfactant-sterile water mixture for dilution. Shake gently for 15 to 20 min to break up clumps of mold. Use a pipet to distribute the mold suspensions evenly over the surface of the greenhouse soil in the tray in the cabinet. 6.3 Allow two weeks of continuous operation for the mold to sporulate and equilibrate with the environment before starting a test. It should not be necessary to recontaminate continually the chamber of panels after sufficient microor ganism growth has built up in the soil, if the chamber is maintained in continuous operation. 6.4 Viability of the mold growth in the cabinet can be checked by placing several malt agar or potato dextrose agar plates,10 open and face up, at several locations on the panel support rods. After 1 h, cover plates and place in incubator at 90 2F (32.5 1C) for 3 days. If an incubator is not available, leave the covered plates in the cabinet. Mold 8 Suitable cultures can be obtained from American Type Culture Collection, 12301 Parklawn Dr., Rockville, MD 20852. Cultures can be maintained on malt agar or potato dextrose agar. Prepared slants can be obtained from Difco Laboratories, Inc., Detroit, Ml 48232; Baltimore Biological Laboratories, Baltimore, MD 21218 or from equivalent sources. 9 Triton X100, Rohm & Haas, Igepal CA-630, GA.E. or equivalent. 10 Prepared agar plates can be obtained from Difco Laboratories, Inc., Detroit, MI 48232; Baltimore Biological Laboratories, Baltimore, MD 21218, or from equivalent sources. 441 DU P050297622 # D 3273 growth should be medium-heavy to heavy and cover the 8. Report complete surface of the agar plate. 8.1 Report the results at the end of the 4-week expose giving the mean and range of the three panels. The resuh from any panel that differs by more than 2 rating units fr0tr| 7. Procedure 7.1 Preparation of Test Panels--Wear disposable plastic gloves or utilize other techniques when handling panels to avoid fingerprints. Prepare triplicate panels by applying two either of the others can be considered manifestly faulty discarded and the mean of the remaining two pan^ reported. If all panels in a set differ by more than 2 units j,, their ratings, discard all results and repeat the test. coats of the material under test to both feces and to all edges 9. Precision and Bias of the panels at a spreading rate of approximately 450 ft2/gal 9.1 On the basis of an interlaboratory study of this | (11 m2/L) per coat or as specified by the coating manufac method in which one operator, in each of seven laboratories turer, allowing 1 day between coats unless otherwise speci rated resistance to mold growth of interior paints at seven fied. Condition the panels at 73.5 3.5F (23 2C) and 50 levels of resistance by visual comparison with photography 5% relative humidity for 4 days after application of the standards, the standard deviations within and between labo. last coat before placing in the test chamber for start of ratories were found to be: environmental exposure. 7.2 Exposure--Hang the panels vertically with the bottom approximately 3 in. (75 mm) above the surface of the Within laboratories Between laboratories Standard Deviations 0.4 units 0.7 units j. Scop* I inoculated soil and with sufficient spacing to allow free circulation of air and to prevent contact between panels or with wall surfaces. Place triplicate panels randomly in the cabinet. Include uncoated control panels in all tests. If the cabinet is operating properly, unpainted panels should de velop a 4 to 6 mold growth rating within 2 to 3 weeks. If this growth is not obtained, the cabinet conditions are not Based on these deviations the following criteria should be used to judge the precision of results at a 95 % confidence level: 9.1.1 Repeatability--Two ratings, each the mean of a set, obtained by a single operator should be considered suspect if they differ by more than 1 unit. 9.1.2 Reproducibility--Two ratings, each the mean of a 1.1 T use with the deg: accumu 1.2 7 ations, . address fffi ft 31 fti ; ?Sy satisfactory or there is some interfering treatment on the panel. 7.3 Rating--Rate the panels for mold growth each week for 4 weeks on a 0 to 10 rating scale using photographic set, obtained in different laboratories should be considered suspect if they differ by more than 2 units. 9.2 Bias--No bias has been determined for this test method. the resi appropr applicai 2. Sign standards (Test Method D 3274). The 50 and 100 magnifi cation photographic standards for types of fungal or dirt 10. Keywords 2.1 1 Iim disfigurement (Test Method D 3274) should be used to confirm the presence of mold as the cause of discoloration. 10.1 environmental chamber; mold; surface interior coat ings paint f disftgur pigmen iirV'-tf The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of tire validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. and alg of as n fungal mende This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadeiphia, PA 19103. 3. Tyi 3.1 3.1. served with t fungi, shown Vr 3.1.: black form attach shown 3.2 Chlori 39x. color. 1 Th Related DO 1.28 Curr publish- 442 DUP050297623 r Designation: D 3274 - 82 (Reapproved 1988)e1 rhe *3 a,,u,ty^ ?, Panels 2 Uns in Standard Test Method for Evaluating Degree of Surface Disfigurement of Paint Films by Microbial (Fungal or Algal) Growth or Soil and Dirt Accumulation1 f 0is te 'oratories ; at seven 'tographie 'een labo. This standard is issued under the fixed designation D 3274; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon <) indicates an editorial change since the last revision or reapprova!. This standard has been approved for use by agencies of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year of issue which has been adopted by the Department ofDefense. <l N()' --Editorial changes were made throughout, including the title, in October 1988. -------------- ------------------------------------:-------------------------------------------------------------------- Jhould be anfldence a of a set, suspect if lean 0f a onsidered this test rior coat- j, Scope 1.1 The photographic reference standards available for tfSe with this test method provide a numerical basis for rating. degree of fungal and algal growth or soil and dirt accumulation on paint films. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to 1 address all ofthe safety problems associated with its use. It is 1 the responsibility of the user of this standard to establish I appropriate safety and health practices and determine the I applicability ofregulatory limitations prior to use. I 2. Significance and Use [ 2.1 The growth of fungi and algae in and on the surface of paint films represents a major cause of discoloration or disfigurement of painted surfaces. Because of their dark pigmentation, it is frequently difficult to distinguish fungi and algae from soil or dirt particles. The use of magnification of as much as lOOx affords easy distinguishability among fungal spores, fungal mycelia, algae, and dirt and is recom mended in cases where such difficulty is apparent. 3. Types of Fungal and Algal Growth 3.1 Two types of fungal growth may be observed: 3.1.1 Spores--Spherical bodies, gray black in color, ob served singly or in clusters. May or may not be associated with fungal mycelia. Spores are the reproductive form of fungi. Spores of Pullularia pullulans magnified lOOx are shown in Fig. 1. 3.1.2 Hyphae--Thread or filament structures, gray to black in color, that make up the mycelium or vegetative form of fungi. Hyphae may appear alone or with spores attached. Hyphae of Pullularia pullulans, magnified 50x are shown in Fig. 2. 3.2 Amorphous growth typical of an alga such as Chlorococcum Sp. appears in Fig. 3 at a magnification of 39x. Terrestrial algae can appear green to dark brown in color. FIG. 1 Spores of Pullularia pullulans, Magnified lOOx FIG. 2 Hyphae of Pullularia pullulans, Magnified 50x 4. Soil or Dirt Particles 4.1 Soil or dirt particles may range from light brown to black. The particles, viewed at 50x to lOOx magnification, are generally amorphous and are frequently translucent. Soil particles on paint magnified lOOx are shown in Fig. 4. 5. Use of Photographic Standards2 5.1 The photographic reference standards that are part of 1 This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DOl .28 on Biodeterioration. Current edition approved Oct. 29, 1982. Published December 1982. Originally published as D 3274 - 73 T. Last previous edition D 3274 - 76. 2 Available from ASTM Headquarters (Request PCN 12-432740-00). Copies of the pictorial photographic standards are contained in the publication Pictorial Standards of Coating Defects, which may be obtained from the Federation of Societies of Coating Technology, 492 Norristown R<L, Blue Bell, PA 19422. 443 DU P0502 97624 6 ?i< i' sS: .1 D 3274 FIG. 3 Amorphous Algal Growth, Magnified 39x this test method are for illustration purposes only and should not be used for evaluation. 5.2 The photographic standards illustrated in Fig. 5 rate the disfigurement of paint films from 0 to 8. A rating of 10 would indicate a film totally absent of disfigurement by particulate matter. 6. Procedure 6.1 Compare each specimen with the photographic stand ards associated with this test method to determine which most closely matches the degree of disfigurement on the specimen. When the degree is intermediate between two adjacent standards select the intermediate odd number as the disfigurement rating. 6.2 The density of fungal or algal growth as well as dirt FIG. 4 Soil Particles on Paint, Magnified 100X accumulation may vary over the painted surface being evaluated. This variation may be the result of the location of the surface (that is, under an eave of a house versus an exposed area), nonuniformity of the substrate, film thickness or other factors. Such variation should be noted when reporting the rating assigned to specimen under test. In examining test specimens for fungal, algal, or dirt disfig urement, the possibility of failure due to the wood substrate should be recognized and reported. 6.3 When microbial disfigurement is detected (or estab lished), distinguish between algal and fungal growth. For the latter, estimate whether spores or mycelia predominate. I 7. Report 7.1 Report the numerical disfigurement rating as defined, in 5.1 and the predominant type, that is, fungi, algae, or soil. i 444 DU P050297625 D 3274 1 FIG. S Disfigurement Ratings The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard-. Users of this standard are expressly advised that determination at the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprovedor withdrawn. Yourcomments are invited either for revision ofthis standardortor additionalstandards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. / 445 DUP05 02 97626 Designation: D 3276 - 86 Standard Guide for , Painting Inspectors (Metal Substrates)1 This standard is issued under the fixed designation D 3276; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval, A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This guide is intended as an information aid to painting inspectors in carrying out their task efficiently. It includes the key elements of surface preparation, coatings application, and final approval for both field and shop work. The items should be selected that are pertinent to the specification of a particular job. N*+' 1--For additional helpful information, refer to the following documents: Manual of Coating Work for Light-Water Nuclear Power Plant Primary Containment and Other Safety-Related Facilities12 New Conceptsfor Coating Protection ofSteel Structures3 SSPC-PA Guide 3 A Guide to Safety in Paint Application4 Steel Structures Painting Manual Vol 1 Good Fainting Practice4 Steel Structures Painting Manual Vol 2 Systems and Specifications4 Manufacturers Specifications and Instructions (made available to the inspector for reference to special requirements for proper application) Material Safety Data Sheets (needed to ensure that personnel take necessary precautions in handling hazardous materials). 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1.3 This guide is arranged in the following order: Section Referenced Documents .............................................................. ASTM Standards .................................................................... OSHA Standards .................................................................... Steel Structures Painting Council Publications ..................... Significance and Use .................................................................. Preparation for Inspection ........................................................ Field and Shop Inspection ........................................................ Surface Preparation ................................................................ Pictorial Standard D2200 ..................................................... Factors Affecting Coating Performance ................................. Cleanliness .............................................................................. Mill Scale ................................................................................ Surface Profile ........................................................................ Cleaning Procedure ................................................................ Chemical Cleaning ................................................................ Solvent Vapor Cleaning ........................................................ Hand Tool Cleaning .............................................................. Power Tool Cleaning................................... ........................ Blast Cleaning ........................................................................ Cleaning and Preparation of Various Surfaces ......................... 2 2.1 2.2 2.3 3 4 5 5.1 5.1.1 5.2 5.Z1 5.2.2 5.2.3 5.3 5.3.1 5.3.1.1 5.3.2 5.3.3 5.3.4 5.4 Steel Surfaces.......................................................................... Galvanized Surfaces .............................................................. Aluminum Surfaces................................................................ Precautions in Preparing Unpainted and Previously Painted Surfaces ............................................................................. Inspection of Surfaces Prior to Field Painting........................... New Construction .................................................................. Maintenance Repainting........................................................ Inspection Equipment................................................................ General ................................................................................. Surface Profile Gages ............................................................ Adhesion of Existing Coating ................................................. Portable Pull-blT Adhesion Testers ......................................... : Field Inspection Equipment .................................................. Drying and Curing Times...................................................... Thermometers ........................................................................ DewPoint ,............................................................................ Coating Consistency .............................................................. Consistency Cups .................................................................. Weight-per-Gallon Cup.......................................................... Wet-Film Thickness Gages .................................................... Interchemical Gage ................................................................ Notched Gage ......................................... ........................... Dry-Film Thickness Gages .................................................... Tooke Gage ............................................................................ Nondestructive Film Thickness Gages ................................... Magnetic-Type Gages ............................................................ Coating Storage and Handling .................................................. Storage of Coating and Thinner ............................................ Mixing of Coatings ................................................................ Thinning ............................................................................... Initial Samples........................................................................ Thinning of Coating .............................................................. Sampling of Thinned Coating ............................................... Heating of Coating ................................................................ Weather Considerations ............................................................ Drying ................................................................................... Low Temperature .................................................................. High Temperature .................................................................. Moisture................................................................................. Wind ..................................................................................... Coating Application .................................................................. Residual Contaminants.......................................................... Quality Assurance .................................................................. Film Defects ......................................................................... Brush Application .................................................................. Spray Application .................................................................. Roller Application.................................................................. Miscellaneous Methods.......................................................... Rate ofApplication :.............................................................. Additional Considerations ........................................................ Ventilation.............................................................................. Shopcoat Repair .................................................................... Painting Schedule .................................................................. Film Integrity.......................................................................... Recoat Time .......................................................................... Coating System Failure.................. .................. ................ Comparison of Surface Preparation Specifications...................... Inspection Checklist .................................................................. Section 5.4.1 5.4.2 5.4.3 5.4.4 5.5 5.5.1 5.5.2 6 6.1 6.1.1 6.1.2 6.1.3 6.2 6.2.1 6.2.1.1 6.2.1.2 6.2.2 6.2.2.1 6.2.3 6.2.4 6.2.4.1 6.2.4.2 6.2.5 6.2.5.1 6.2.6 6.2.6.1 7 7.1 7.2 7.3 7.3.1 7.3.2 7.3.3 7.4 8 8.1 8.2 8.3 8.4 8.5 9 9.1 9.2 9.2.1 9.3 9.4 9.5 9.6 9.7 10 10.1 10.2 10.3 10.4 10.5 10.6 Table 1 Appendix 1 This guide is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.46 on Industrial Protective Coatings. Current edition approved Sept. 29, 1986. Published November 1986. Originally published as D 3276 - 73. Last previous edition D 3276 - 73. 2 AST14.1979. 2 ASTM STP 841, ASTM, 1984. 4 Available from Steel Structures Painting Council, 4400 fifth Ave., Pittsburgh, PA 15213. 2. Referenced Documents 2.1 ASTM Standards: D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers5 5 Annua/ Book ofASTM Standards, Vol 06.01. 446 D1 E ti D1 0 D1 E P D1 q D1 n D2 n D2 F D3 1 D3 C D4 C D4 t D4 F D4 l E2 r 2.2 (OSh Ha 2.3 SSI SS) SSI SS SS SS SS SS SS SS SS ) 3. Si 3.! ceme punc Man; parti. 6 A, 7 A. SA Office. DUP050297627 Section 5.4.1 5.4.2 5.4.3 5.4.4 5.5 5.5.1 5.5.2 6 6.1 6.1.1 6.1.2 6.1.3 6.2 6.2.1 6.2.1.1 6.2.1.2 6.2.2 6.2.2.1 6.2.3 6.2.4 6.2.4.1 6.2.4.2 6.2.5 6.2.5.1 6.2.6 6.2.6.1 7 7.1 7.2 7.3 7.3.1 7.3.2 7.3.3 7.4 8 8.1 8.2 8.3 8.4 8.5 9 9.1 9.2 9.2.1 9.3 9.4 9.5 9.6 9.7 10 10.1 10.2 10.3 10.4 10.5 10.6 Table 1 Appendix Dry-Film eters5 D 3276 p 1186 Test Methods for Nondestructive Measurement of Dry-Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base5 p 1212 Methods for Measurement of Wet Film Thickness of Organic Coatings5 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base5 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products5 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting6 P2092 Practices for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Painting5 D 2200 Pictorial Surface Preparation Standards for Painting Steel Surfaces5 D3359 Test Methods for Measuring Adhesion by Tape Test5 D3843 Practice for Quality Assurance for Protective Coatings Applied to Nuclear Facilities5 D4212 Test Method for Viscosity by Dip-Type Viscosity Cups5 D4414 Practice for Measurement of Wet Film Thickness by Notch Gages5 D4417 Test Methods for Field Measurement of Surface Profile of Blast Cleaned Steel5 D4541 Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers3 E 376 Practice for Measuring Coating Thickness by Mag netic-Field or Eddy-Current (Electromagnetic) Test Methods7 2.2 Occupational Safety and Health Administration (OSHA) Standard: Hazard Communication8 2.3 Steel Structures Painting Council Standards:4 SSPC-SP 1 Solvent Cleaning SSPC-SP 2 Hand Tool Cleaning SSPC-SP 3 Power Tool Cleaning SSPC-SP 5 White Metal Blast Cleaning SSPC-SP 6 Commercial Blast Cleaning SSPC-SP 7 Brush-off Blast Cleaning SSPC-SP 10 Near-White Blast Cleaning SSPC-PA 1 Paint Application Specifications SSPC-PA 2 Measurement of Paint Thickness with Mag netic Gages SSPC-Guide to Vis 1 Pictorial Surface Preparation Standr ards for Painting Steel Surfaces SSPC-Paint 27 Basic Zinc Chromate-Vinyl Butyryl Wash Primer 3. Significance and Use 3.1 This guide is intended as a reference for those con cerned with the inspection of industrial coating work. A punch list for use in the field is included as an appendix. Many of the details covered may be in a specification for a particular project. A specification for coating projects should 6 Annual Book ofASTM Standards, Vols 02.05 and 06.01. .. ' Annual Book ofASTM Standards, Vols 01.06 and 03.03. 8 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. include the coatings to be used. The various items are explained in detail in the appendix. 4. Preparation for Inspection 4.1 The guide describes the duties of the inspector and discusses inspection methods, both visual and instrumental, that can be used to determine that the specification require ments have been met by the painting contractor. 4.2 Before painting is started the project engineer must provide the inspector with information from the official plans and specifications as to coating type, thinner to be used, mixing ratios to be used, recommended application thickness, recommended primer, tie coat, topcoat, time between coats, surface preparation, method of application, and any special precautions to be followed such as limits on ambient conditions. These details should be recorded in an inspector's record book to eliminate any misunderstanding between the inspector and the contractor. 5. Field and Shop Inspection 5.1 Surface Preparation is one of the most important factors affecting the performance of coatings. The specifier should determine the proper level in accordance with the expected service life and type of coating specified. 5.1.1 Pictorial Standard D 2200 (SSPC-Vis 1) should be provided to the inspector on a job involving painting of structural steel. The standard is used by the inspector to determine whether the degree of surface preparation speci fied in a contract has been attained by the contractor. For large jobs it is recommended that before work starts, an actual steel sample of adequate size be blasted to the satisfaction of the project engineer. This blasted surface should be protected by a clear acrylic coating or encased in plastic and used for reference purposes as the work progresses. 5.2 Factors Affecting Coating Performance--There are a number of factors that must be considered to ensure a proper painting job. 5.2.1 Cleanliness--Many materials if not removed from the surface will affect the life of the coating. These include oil, grease, soil, weld spatter, and slag that make it impossible to obtain proper adhesion to the metal surface. Deposits of salts (such as chlorides and sulfates) must be removed or long-term coating performance will be seriously affected. The Steel Structures Painting Council (SSPC) issues detailed surface preparation specifications that cover methods for solvent cleaning and hand and power tool cleaning as well as the various methods of blast cleaning. 5.2.2 Mill Scale, the bluish-black oxide resulting from the hot-rolling process, is a constant source of trouble leading to coating failure. This scale is very hard and can crack or loosen from temperature changes both in fabricating and weathering in the field. 5.2.3 Surface Profile--The texture of the metal surface has a significant effect on the performance of coatings since it increases the surface area to which the coating can develop adhesion. In fact, the term "anchor pattern" is sometimes used to describe the depth of profile required. This varies both with the type and size of the abrasive used. Coarser abrasives generally produce a coarser and deeper profile. Deep profiles are advantageous for adhesion but require 447 DU P050297628 # D 3276 l more coating to fill in the valleys and cover the peaks of the profile; they cannot be used with low-build coatings that do not cover the peaks even when several coats are applied. A general recommendation is that the surface profile should be one quarter to one third of the dry film thickness of the coating system but does not apply in every case if the resulting profile would be too great. . 5.3 Cleaning Procedures--Safety precautions are not ad dressed separately for each of the following cleaning methods. Each has its own safety-related hazards, and U.S. Occupational Health and Safety Administration regulations should be followed. Material Safety Data sheets (MSDS) for the solvents and cleaning compounds provided by the manufacturer should also be consulted for proper worker protection. 5.3.1 Chemical Cleaning--Solvents are used to remove oil, grease, and related materials. The solvent is applied to the surface by wiping or scrubbing with rags or brushes. The contaminants must be removed (not simply spread out) by a thorough wiping of the affected areas with cloths saturated with clean solvent. Contaminated cloths must not be dipped into clean solvent. The cleaning should be repeated with clean rags and fresh clean solvent. Emulsions, cleaning compounds, steam cleaning, or similar methods and mate rials may also be used. Where emulsion cleaners, soaps, or detergents are used, they must be removed completely by washing with clean hot water. SSPC SP-1 covers cleaning procedures using these materials. 5.3.1.1 Solvent Vapor Cleaning is a procedure that can be adapted to a production line or a piecework operation. Vapor cleaning removes all soluble contaminants but does not disturb the natural oxide film. If this film must be removed, mechanical cleaning will be necessary as well. The part to be cleaned is placed in the saturated vapor above the heated solvent so that the solvent vapor condenses on the metal surface. Vapor degreasing does not remove particulate matter and parts must be wiped to remove any insoluble; soils. Vapor degreasing has the advantage over solvent wiping in that hot solvents .are used and the solvent condensation removes soils without recontamination. 5.3.2 Hand Tool Cleaning is the method used for the removal of loose mill scale, loose rust, loose or otherwise defective coating, weld flux, slag and spatter from metal surfaces by hand brushing, hand sanding, hand chipping or scraping using wire, fiber, or bristle brushes, sandpaper, steei wool, hand scrapers or chisels, and chipping hammers. The surface is then cleaned to the condition St 2 given in Method D 2200 (SSPC-Vis 1). SSPC also provides a detailed specifi cation, SSPC-SP 2. 5.3.2.1 Hand tool cleaning requires that all tar, oil and grease, weld flux, and other greasy contaminants be removed TABLE 1 Comparison of Surface Preparation Specifications Preparation Grade SSPC ^ ASTM D2200 NACE Blast cleaning to white metal Blast cleaning to near-white Commercial blast cleaning Brush-off blast cleaning SSPC-SP 6 SSPC-SP 10 SSPC-SP 6 SSPC-SP 7 Sa 3 Sa2 Vz SaZA Sal 1 2 3 4 4 Pictorial standard B Sa 2-Vi shows mill scale and conflicts with the SSPC definition of commercial blast (SP6) which does not allow mill scale. first by solvent cleaning (5.3.1). gurfec 5.3.2.2 Wire brushes should be rigid enough to clean th surface thoroughly and shaped to penetrate into all cortie>! clean pjoisti and joints. Brushes should be kept free of all materials that produ may clog the wires of the brush. Hand scrapers should be made of tool steel, tempered and ground to a sharp edge and rerno' 5.3- should be of the proper size and shape to enable cleaning t0 prinie be done as specified. Scrapers should be kept sharp at ah times. 5.3.3 Power Tool Cleaning is a method used for the blasts visibl Surfa< removal of loose mill scale, loose rust, loose or otherwise 5-4 defective coating, and weld flux from metal surfaces by power wirebrushes, power impact tools, power grinders power sanders, or by a combination of these methods. The pefoJ rnust requi surface is cleaned to the condition St 3 given in Pictorial tools Surface Preparation Standards D 2200. SSPC-SP 3 is the detailed specification for power tool cleaning. ItlOV' shou 5.3.3.1 Power Tool Cleaning requires that all oil, grease ratec weld flux, and other contaminants be removed first by dripi solvent cleaning (SSPC-SP 1). Hand tool cleaning in accordance with 5.3.2 may be used prior to power tool cleaning. ical stru< 5.3.3.2 All equipment must be suitable for the confignra. acce tion of the work to be cleaned and maintained free of 5. material that clogs the wire or disks making them ineffective. don All impact tools should be kept sharp. pow 5.3.4 Blast Cleaning is used to remove foreign materials 5 from a metal surface and to provide a roughened surface by fror striking the surface with a stream of small, hard abrasive The particles such as (dry) sand, grit, or shot. the 5.3.4.1 One method utilizes compressed air, special blast atte nozzles, and abrasive. In another method used in a fabri poc cating shop, wheels propel the abrasive centrifugally against cle; the work. The minimum and maximum particle size of the cle. abrasive may be specified as a means of controlling the adl - surface profile. Water may be injected into the air stream to me control dust. Occasionally a high-pressure water blast, either rin with or without an abrasive injected into the stream, is used as an alternative to open blasting since it reduces the release cle of dust into the atmosphere. Pr 5.3.4.2 Blast cleaning requires that all oil, grease, and weld to flux be removed by solvent cleaning. The compressed air p; used for blast cleaning should be free of condensed water or oil by making certain that separators and traps are in working order. t u 5.3.4.3 Blast-cleaning operations should be performed so d- that no damage is done to the completed portion of the s< work. Blast cleaning is often performed from the top to w bottom of the structure and should only be carried on P downwind from any recently painted areas. Dry blast cleaning operations should not be conducted on surfaces that, P will be wet after blasting and before painting. Dew point'| must be at least 5F (3C) above the steel temperature. 1 Iv 5.3.4.4 The degree of blast'cleaning required should a|j V least be equal to the appropriate SSPC surface preparations | | I specification and the applicable pictorial standard shown aW3f ! Pictorial Surface Preparation Standards D 2200 (SSPC-Vis 1) r or National Association of Corrosion Engineers (NACE) as j shown in Table 1. 5.3.4.5 Blast cleaned surfaces must be examined for any traces of oil, grease, or smudges; where present, the contam inants must be removed by solvent cleaning (see 5.3.1)- > DUP050297629 the 3rners s that ild be te and agio at all r the Jrwise es by aders, The ;torial is the tease, 'st by -'cord ing, iguraee of ictive. terials ice by rasive 1 blast fabrigainst of the tg the am to either 5 used elease weld d air er or e in ed so jf the op to :d on blast :s that point old at ration wn in Vis 1) :E) as ir any ntaffl5.3.1)- 0 3276 .uffaces that have been dry blasted should be brushed with s brushes, blown with compressed air free of oil and pjsture, or vacuum cleaned to eliminate any traces of blast ^oducts, dust, or dirt from the surface. This also serves to Unlove abrasive from pockets and comers. 11 j 3.4.6 Blast cleaned surfaces should be further treated, ,ijned or painted as specified on the same day they are pasted, preferably within 8 h, or in any event before any yjsjble rerusting occurs. Reblasting will be necessary on any (iicface if rust bloom forms before the coating can be applied. 5,4 Cleaning and Preparation of Various Surfaces-- Before application of any coating, all surfaces to be coated pjst be thoroughly cleaned and properly prepared to the j^quirements of the specification. All dust, dirt, oil, grease, jjoisture, soot, tars, or other contaminants should be re moved from unpainted surfaces. Previously painted surfaces jjjould be similarly cleaned of all foreign matter; all deteriomted coating must be removed as well. Mortar or cement (jrippings from earlier repairs must be removed by mechan ic or chemical means. Tree limbs or other growth ob structing the structure should be cut away to provide ready access. 5.4.1 Steel Surfaces--Removal of rust and scale must be done in the manner and to the degree specified, that is, hand, power tool, or blast cleaned. 5.4.1.1 On bridges, all dirt and debris must be cleaned Jem around bearing plates, shoes, and other components. The entire surface of the beam or truss seat on each unit of the structure should be cleaned. On truss spans particular attention should be paid to removal of dirt and debris from pockets and crevices. Open steel grid-type decking should be cleaned by use of a detergent steam-water-type jet that will clean painted surfaces without softening or removing tightly adhering coating. The machine manufacturer's recom mended solution should be used. Surfaces should then be nosed with a clear water jet. 5.4.2 Galvanized Surfaces that are to be painted should be cleaned and treated in accordance with Method A or D of Practices D 2092. Alternatively, the surface may be allowed to weather a minimum of 6 months before cleaning and painting. 5.4.3 Aluminum Surfaces: 5.4.3.1 Complete removal of oil and grease and, for unanodized aluminum, treatment is essential. Vapor degreasing or immersion in an alkaline or acid cleaning solution are commonly used in shop work. In the field a water wash followed by solvent cleaning is a good starting point. 5.4.3.2 Vinyl wash primer is one of the metal pretreatments commonly used on unanodized aluminum. The material is described in Practices D 1730, Type B, Method 8 and is covered by SSPC Paint 27. For exterior work an inhibitive primer is required over this pretreatment, head pigmented primers should never be used over alu minum surfaces. The minimum treatment for aluminum is Type B, Method 3 of Practices D 1730, which describes the use of an alcoholic phosphoric acid cleaner. 5.4.4 Precautions in Preparing Unpainted and Previously ^dinted Surfaces--Cleaning should proceed by sections, tays, or other readily identifiable parts of the work. The 'leaning of each section, bay, or part of the work must be entirely completed, inspected, and accepted before any coating is applied. The system of alternately cleaning and painting short sections by one workman is not good practice. 5.4.4.1 If, in the opinion of the project engineer, traffic, or any other source produces an objectionable amount of dust, it is customary for the contractor, at his own expense, to control the dust by using tarpaulins, etc., for a sufficient distance around the structure and take any other precaution necessary to prevent dust and dirt from coming into contact with the cleaned or freshly painted surfaces. It may some times be necessary between the various coats to clean newly coated surfaces using some of the specified methods. 5.4.4.2 Some areas to be painted or repainted are exposed to chemical fumes and should be washed with water before painting. Washing may also be necessary between coats of paint. If there is reason to suspect the presence of chemicals, the surfaces should be tested before applying subsequent paints. 5.4.4.5 Residual contaminants present on pitted steel can be a problem. Chloride from deicing salts or a marine environment and sulfate contamination from air pollution have recently been recognized as one of the main factors in premature breakdown of coating systems. High-pressure water blasting is often used to remove these contaminants. 5.5 Inspection ofSurfaces Prior to Field Painting: 5.5.1 New Construction--It must be emphasized that the first coat should be applied to the cleaned surfaces before any soiling or deterioration can occur. If painting is done out of doors, the cleaned areas should receive the first protective coat well before nightfall brings lower temperatures and possible moisture condensation on the surfaces. When sur face preparation and painting are carried on indoors, over night delays between cleaning and painting may be permis sible except on blast-cleaned surfaces. 5.5.1.1 Shop-coated steel that has been shipped to the erection site should be stored on blocks to prevent contact with the ground and where it is least likely to be marred, scratched, or subjected to harmful contamination by grease, oil, salts, etc. Insofar as practicable, the steel should be stored to avoid the formation of waterholding pockets. If outdoor storage lasts for several months, the inspector should check the integrity of the coating from time to time, and have any deficiencies corrected. Correction of these deficiencies may require complete blast cleaning and repriming in the field if the shop primer has weathered so long as to make touch up too extensive. The length of time between shop priming and erection and subsequent topcoating should be kept to a minimum to avoid the problem of intercoat adhesion. 5.5.1.2 Immediately before applying the first field coat, the shop-coated surfaces should be cleaned of dust. If necessary to remove grime and oil substances, they are wiped with solvents selected so as not to soften the film appreciably. Miscellaneous scratches and breaks in the shop coat, in cluding those occasioned by field welds, bolts, or rivets, should be cleaned and touched-up as specified before the steel receives the first overall field coat 5.5.1.3 The inspector must ensure that field rivets have been cleaned of slag and weld spatter. It is important that every coat of the system be applied over dry, soil-free surfaces, and that all previous coats be free of mechanical damage. Great care should be exercised to prevent trapping 449 DUP0502 97630 0 3276 corrosive salts under or between coats. 5.5.1.4 The inspector should determine whether the spec ifications are being followed with reference to the painting or prohibition of painting of contact surface's in bolted or riveted surfaces of construction. He must ensure that sur faces not in contact but that will be made inaccessible by assembly or erection, have received the full number of specified coats before they become inaccessible. 5.5.2 Maintenance Repainting--In most cases, mainte nance painting will consist of spot-cleaning and priming of small isolated areas of deterioration followed by application of one overall new finish coat to all surfaces of the structure. The inspector of maintenance painting must be alert for several conditions not encountered in the painting of new work. 5.5.2.1 Sound coating not intended to be removed should not be damaged by cleaning operations on adjacent areas. This is particularly important with spot-blast cleaning. 5.5.2.2 The junctions between sound coating and spotcleaned areas should present a smooth, feathered appear ance. The application of coating to spot-cleaned areas should overlap the old, adjacent coating to a slight extent in order to assure full coverage of the cleaned areas. Before the overall finish coat is applied, the inspector must ensure that oil, grime, dust, and other contaminants are cleaned from the old coating surfaces. 5.5.2.3 Before work has progressed too far, adhesion of the newly applied coat to the old coating should be carefully checked. Under the direction of the engineer the inspector may explore beneath the surface of the existing or new coating film for covered-over rust or loosening of the old film, and where he discovers such conditions, require that the surface be cleaned and repainted. 5.5.2.4 The effect of any newly applied coating on the old underlying coating should be noted. Any coating that shows curling, lifting, or excessive wrinkling should be reported to the engineer immediately since it may have to be removed and the area repainted. If the defects are general, rather than existing in a few isolated areas, use of a different type of coating may be necessary. 6. Inspection Equipment 6.1 General--Visual observation is the most important part of inspecting coating application. There are, however, instruments and mechanical aids that are of considerable help to the inspector. They make the painter aware that his work can be checked during progress and even after comple tion. The different instruments that can be used are de scribed in this section. 6.1.1 Surface Profile Gages--The inspector can determine the surface profile of blast-cleaned steel substrates using Test Methods D 4417 to assure an adequate "tooth" is obtained for the specified material. Some of the common instruments are: 6.1.1.1 Surface profile comparator9 for visual compari sons of the profile against a reference disk for sand, grit, and shot blast-cleaned steel. 6.1.1.2 Depth micrometers with conical points to project into the valleys to determine profile depth. 6.1.1.3 Tape,10 to create an exact replica of the profile on a special material. The tape is measured in the field using a spring micrometer to determine average maximum profile height. 6.1.2 Adhesion of Existing Coating--The inspector should carry a pocket knife that can be used to determine the soundness of existing paint where there might be blistering or underfilm corrosion. This is a subjective test and its value depends upon the inspector's experience. The cross-cut test, Methods D 3359, is more reproducible. 6.1.3 Portable Pull-offAdhesion Testers are available. The apparatus measures the force required to remove a metal stud that has been cemented to the coated surface as described in Method D 4541. 6.2 Field Inspection Equipment in good working order should be available to the inspector so that he may perform his function properly. 6.2.1 Drying and Curing Times--These are both imporfant considerations since drying time and curing time can both be affected. Minimum temperatures are required for reactive and water-borne coatings while too high a tempera ture can make application difficult. Inorganic zinc-rich primers and moisture-cure urethanes require certain min imum humidity conditions for proper cure. The manufactur er's recommendations must be followed. 6.2.1.1 Thermometers--The paint inspector may need several types of thermometers and should have at least an accurate pocket thermometer with a range from about 0 to 150F (--18 to 65C) for measuring the ambient air temper ature. The same thermometer or a floating dairy thermom eter may be used to determine the temperature of liquid coating, solvent, etc. The pocket thermometer may also be used for determining the temperature of metal surfaces by placing it against the metal while shielding the outer (away from the metal) side of the bulb by means of putty or similar material, so that the reading is not affected by the ambient temperature. Flat surface-temperature thermometers are also available for this purpose. 6.2.1.2 Dew Point--A psychrometer containing a wetand dry-bulb thermometer for determining relative humidity and dew point is a useful inspection tool. Hand-held sling or electrical types are available as well as a direct reading digital type. 6.2.2 Coating Consistency is an important characteristic since durability is related to film thickness and whether a film of the proper thickness can be applied is partly controlled by consistency. 6.2.2.1 Consistency Cups--There are occasions, such as on-site thinning, when it is necessary to check paint consis tency during field application. While giving only partial information about the viscosity of a coating, the Zahn cup is a portable device for checking quickly the approximate consistency of coatings and other liquids. It consists of a bullet-shaped, stainless steel cup with an orifice in the bottom. Attached to the cup is a looped handle with a small 9 Comparator, manufactured by ICeane-Tator, l E 5 Technology Dr. Pittsburgh, PA 15275 has been found satisfactory for this purpose. 10Press-O-Fflm tape; manufactured by Tcstex, has been found 'suitable for this purpose. 450 ring at withdra cup is c. vvithdra the liqu viscosir be note; have po is poor- 6.2.3 inspect; paint ir specific, been d< show tl applicai tity of temper; has a cl is filled As the ; and is i and w< sensitiv ence be weight for the 6.2.4 ment if paint ii erronec fast-dn used tc first, g underc reading softeni: be use; results 6.2.- over tl the si (micro Metho 6.2.- brated the pre then w The tr coated proced 6.2,,` measu tion of coating nonde; trating needle betwee dimen an att; DUP050297631 "oject leon ;inga rofile 'ector e the ng or value : test, The tietal 'e as order form tpor: can d for pera>rich minctur- need st an 0 to nper10miquid ;o be ;s by away nilar bient also vetlity ; or ,ital ristic ler a artlv :h as msisartial up is mate of a the small or this D 3276 11 ; -jjg at the top to align the cup in a vertical position when : ^drawing it from the liquid being tested. To operate, the cUp is completely immersed in the liquid to fill it and is then withdrawn rapidly and completely. The time in seconds for This type of gage destroys the film at the inspection points, necessitating touch up with primer and finish to prevent corrosion at these spots. One kind of cutting gago is described in 6.2.5.1. jjje liquid to escape through the orifice is an expression of 6.2.5.1 Tooke Gage--The Tooke inspection gage is de viscosity, that is, Zahn Cup No.( ) seconds. It should signed to measure coating film thickness by microscopic noted that Zahn cups are not suitable for all coatings and observation of a cut into the film. The tungsten carbide Mve poor reproducibility (agreement between different cups cutting tip is specially shaped to slice a precise narrow groove jSpoor--see Test Method D 4212). through a film and into the substrate at an angle to the 6.2.3 Weight-per-Gallon Cup--There are times when the surface. Thickness of coating on any type of stable substrate inspector may wish to check the weight-per-gallon of the may be determined and individual coats may be measured paint in the field. If the value is low compared to the paint separately providing they are distinguishable, for example, by specification, it indicates that unauthorized thinning has color. The coating cannot be too brittle or soft, otherwise the ijeen done, while differing values from the same container cutting tip will tear rather than precisely cut through the show that the coating has not been thoroughly mixed for coating, making accurate readings impossible. application. The weight-per-gallon cup holds a given quan- 6.2.6 Nondestructive Film Thickness Gages are widely jity of water when filled at 77F (25C) or other specified tefflPerature- ft is made of corrosion-resistant material and has a closely fitted lid with a small hole in it. In use, the cup used for field and shop inspection. For ferrous metals they are based on magnetism, and for nonmagnetic metals on inductance and eddy currents. There are no satisfactory jS filled with liquid slightly below the specified temperature. As the contents warm up, the excess escapes through the hole and is removed. The filled cup is wiped clean on the outside and weighed. A relatively inexpensive balance having a sensitivity of 0.1 g provides sufficient accuracy. The differ ence between the full and empty weights divided by 10 is the weight in pounds of 1 gal of the paint. Complete instructions for the procedure are given in Test Method D 1475. 6.2.4 Wet-Film Thickness Gages--This type of instru ment is designed to measure the thickness of a wet film of paint immediately after it is applied to a surface. Note that erroneous readings may result when using the gage on fast-drying paints such as inorganic zinc. If a wet-film gage is used to determine the thickness of coats subsequent to the first, great care must be taken that partially hardened undercoats are not indented by the gage, thus giving high readings. If the coat being measured has an appreciable softening effect on the previous coat, a wet-film gage cannot be used with accuracy. It is very important to record test results and send a copy to the engineer. 6.2.4.1 Interchemical Gage--This instrument is rolled over the newly applied wet film on a smooth flat portion of the surface and the thickness read directly in mils (micrometres). Complete details are given in Method A of Methods D 1212. 6.2A.2 Notched Gage--This device has a series of cali brated steps for measuring thin to heavy coats. The gage with nondestructive methods for wood or other nonmetallic substrates. All of the different types require calibration with standards the thickness of which is known and in the same range as the coating to be measured. The calibration must be made on metal of the same kind, temper, thickness, and contour as that beneath the coating. Test Methods D 1186 and 1400 describe procedures. Measurements on relatively rough surfaces, such as a surface blasted to a high profile, may be misleading unless the instrument is calibrated on an identical surface. 6.2.6.1 Magnetic-Type Gages'1--Use either an electro magnet requiring a power supply or a permanent magnet. The principle of the method is that a nonmagnetic coating changes the magnetic force between the magnet and the magnetic base or the magnetic flux between the poles of the magnet. As the change is a function of distance from the metal, the gage can be made to read film thickness directly. Magnetic gages may be affected by the mass of the steel, or if electric welding is being carried out on a structure, for example, a ship's hull, at the time of measurement. Test Methods D 1186 describe the procedure for using magnetic gages. The method is also described in SSPC-PA 2 which includes instructions on the number of measurements for different areas and tolerances on the required film thickness. 6.2.6.2 Nondestructive procedures based on inductance and eddy current techniques are described in Test Method D 1400. the proper face is placed squarely on the fresh, wet film. It is then withdrawn perpendicularly without a sliding movement. 7. Coating Storage and Handling The true wet-film thickness lies between the highest step coated and the next highest which was not coated. The procedure is described in Practice D 4414. 6.2.5 Dry-Film Thickness Gages--Dry-film thickness measurements are of great importance because the protec tion of the substrate is directly related to the thickness of the ! coating. There are two ways of making the measurements, i nondestructive^ or destructively. The latter involves pene- 7.1 Storage of Coating and Thinner--All coatings and thinners should be stored in areas or structures that are well-ventilated and not subject to excessive heat, open flames, electrical discharge, or direct rays of the sun. Storage should be in compliance with applicable regulations. Mate rials susceptible to damage at low temperatures must be stored in heated areas. If a coating is stocked for a consider- ; bating or cutting through the film to the substrate with a needle or blade and measuring by some means the distance between the top and..bottom of the film. Because the dimensions are so small, some cuts are made at an angle in an attempt to increase the accuracy of the measurement. 11 Type /--Pull-offgages (such as Mikrotest, Inspector ThicknessGage, and the Pencil Pull-Off Gage, or, Tinsley, type gage); and.Type 2--F,ixed Probe Gages (such as ElcOmeter Thickness Gage, Miiutector, General Electric Type B Thickness Gage, Verimeter, Permascope, Dermitron, Positector, Certotest, Accuderm and Minitest) have been found suitable for this purpose. 451 ii ( DU P050297632 D 3276 able length of time (several months), it is desirable to invert the containers at monthly intervals. This will prevent hard settling and thus make mixing quicker and easier when the coating is to be used. 7.1.1 Coating containers should remain unopened until needed and the oldest should be used first. The manufactur er's written instructions should be followed regarding shelf life. Coatings that have livered, gelled, or otherwise deterio rated during storage should not be used. If a particular material is in question, do not use it until it has been tested by the manufacturer or independent laboratory and found to be satisfactory. 7.1.2 Where a skin has formed in the container, the skin should be cut loose from the sides of the container, removed and discarded. If it is felt that the skins are thick enough to have a practical effect on the composition, the remaining paint should not be used until it has been tested and found to be satisfactory. 7.2 Mixing ofCoatings--All coatings must be thoroughly and completely mixed in clean containers before use. Where there is noticeable settling and mixing is done either by power stirrers or by hand, most of the vehicle should be poured off into a clean container. The pigment is then lifted from the bottom of the container with a clean broad, flat paddle, lumps broken up and the pigment thoroughly mixed with the vehicle present. The poured-off vehicle should be returned slowly to the original container with simultaneous stirring. It is also useful at this point to mix or pour repeatedly from one container to another (boxing) until the composition is uniform. The bottom of the original con tainer should be inspected for unmixed pigment. The coating should not be mixed or kept in suspension by means of an air stream bubbling under the coating surface. 7.2.1 Some coatings may require straining after mixing to ensure homogeneity and to remove skins and foreign matter. The strainers should be of a type to remove only skins, etc., but not to remove pigment. For example, a 150-mesh (105-pm) strainer is normally satisfactory for most coatings unless some specific size is required in the specification. Coatings should not remain in buckets, spray pots, etc., overnight, but be gathered into a container and remixed before use, provided the manufacturer's stated pot life will not be exceeded. Containers must be covered when not in use, to reduce volatile losses and skinning. 7.2.2 Coatings should be agitated enough during applica tion to ensure homogeneity. Some materials may even require constant agitation during use. 7.3 Thinning--Some specifications permit field thinning of laboratory-accepted coatings while others do not. This section describes some commonly accepted procedures when thinning is permitted. 7.3.1 Initial Samples--When thinning on the job site is permitted and unless other arrangements have been made, (for example using manufacturer-supplied thinner from unopened containers and complying with manufacturer's written thinning instructions), the painting inspector may need to submit to an agreed-upon testing laboratory a 1-qt (1-L) sample from each batch to be thinned, together with a 1-qt sample of the thinner to be used using clean sample containers in both cases. With these samples a request is submitted for advice on the proper thinning rate for the conditions prevailing and the consistency limits of . thinned coating. 7.3.2 Thinning ofCoating--Ml additions ofthinner mu,. be made in the presence of the inspector and no othe amounts or types of thinner than those permitted by tj specification or manufacturer, or both, may be added Thinning is carried out by pouring about half of th thoroughly mixed coating into an empty, clean container The required thinner is then added and the two portions are boxed to obtain a homogeneous mixture. 7.3.3 Sampling of Thinned Coating--During the work additional samples need not be submitted for testing unless a deviation is noted in the coating consistency or if it suspected that there has been a change in the thinner. 7.3.3.1 When an inspector is qualified and has the necessary equipment available at the field office, arrangements may be made for on-site inspection of thinning and of the thinned coating. This speeds acceptance of a coating and lightens the laboratory workload. The inspector must keep a record of all paint modifications, amount of thinning, weight per gallon, and viscosity. Where dry-film thickness is speci fied, the inspector must calculate the new wet thickness necessary to obtain the desired dried thickness with the thinned coating. He should make frequent checks ofwet-filtu thickness as work progresses, however compliance with the specification should be based on dry-film thickness where possible. 7.3.3.2 To determine the wet-film thickness of the thinned coating required to obtain the specified dried-film thickness, the percent volume of nonvolatile (solids) in the original coating must be known. This figure is readily obtained from the manufacturer. With this information the calculation may be made as follows: ! W= D (1.0 T)/S where: W - wet-film thickness, D = desired dry-film thickness, S - percent by volume of coating solids, and T = percent by volume of thinner added. 7.4 Heating of Coating--Coatings as delivered in the manufacturer's containers and mixed thoroughly, are ready for use, unless the specification permits on-site thinning of high-viscosity material. Should the coating temperature be low, that is, 50F (10'C) its consistency may increase to the point where application is difficult. Where thinning is not permitted, the coating may be heated. Should the contractor wish to reduce the viscosity by heating to make application easier, the containers may be warmed in hot water, on steam radiators, or by other acceptable indirect heating processes, In-line heaters are also available for application equipment. Direct application of flame to the containers is forbidden by fire regulations. It should be noted, however, that heating of the coating alone will not compensate for ambient or surface temperatures, or both, that are below the minimum specified for that material. prote 8.2 perat eithe temp syste abov pain drop solvt (0C com penc dry. fail* 8. face that that film whe the 8 sno sur spr sur spe ust anc sus sue ins to CO! wi' aci (3` lig e\ ei to di W' Pi sa c< e> n d si o 8. Weather Considerations 8.1 Drying---It is well known that most coatings, particularly those for structures, will not dry properly at low temperatures and high relative humidities, nor will they o n a 3 c 452 DUP050297633 of the er itlUst 0 Qther by the ad<iecL % ntamer ions ^ 2 work, unless a if it is r. 2 neces;ements i of the ng and keep a weight s speciickness ith the ret-film nth the where of the ed-film in the readily ion the i the eady ig of e be o the s not tractor ication steam cesses, jment. den by ting of iurface etified articuit low 1 they D 3276 tect if applied owr wet surfaces. P ^2 Low Temperature--Many specifications indicate tem- `tUre limits between which painting may be undertaken ^her in the shop or in the field. The minimum ambient c' erature is usually 40C (5C) or for cold-curing epoxy SOT (10C) with the temperature of the substrate 5Lve freezing. The requirements may state further that Ljating should not be undertaken when the temperature is topping. However, some authorities believe that many ^[vent-borne coatings may be applied at (or below) 32F without adverse effects. Within the limitations of the composition of the coating, this may be satisfactory de luding upon the type ofcoating and providing the surface is Painting over ice or frost will result in early adhesion failure of the coating. g.3 High Temperature--The maximum reasonable sur face temperature for application is 125F (50Q. A surface djat is hot may cause the coating solvents to evaporate so fast that application is difficult, blistering takes place, or a porous gm results. To keep the temperature down it is desirable, where practical, to paint under cover at a shop or to protect the surfaces from the sun with tarpaulins. g.4 Moisture--Painting should not be undertaken in rain, snow, fog, or mist, or when the temperature of the metal surface is below the dewpoint. This is especially true in the spring and fall when days are warm and nights are cool. Wet surfaces should not be painted unless the coatings are specifically designed for that condition. Relative humidity is usually a good index of the acceptability of air conditions and specifications often contain an 85 % upper limit. If it is suspected that the temperature and humidity conditions are such that moisture is condensing upon the surface, the inspector may make the following test: Use a psychrometer to determine the actual relative humidity and dew point; compare the dew point with the metal temperature measured with a surface temperature thermometer. It is generally accepted that the surface temperature should be at least 5F (3C) higher than the dew point. A less accurate test is to lightly moisten a small area with a damp cloth and observe. evaporation and drying; if the dampness decreases and evaporates within 15 min, the surface is considered satisfac tory for the application of coating from the standpoint of dampness and condensation at that particular time. 8.4.1 When coatings must be applied in damp or cold weather, the substrate should be painted under cover, or protected from the surrounding air, and the steel heated to a satisfactory temperature. The steel should remain under cover until dry or until weather conditions permit its exposure in the open. 8.4.2 Applied coatings exposed to freezing, excessive hu midity, rain, snow, or condensation should be permitted to dry. Damaged areas of coating should then be removed, the surface again prepared and painted with the same number of coats of the same kind as the undamaged area. 8.5 Wind--The wind direction and velocity must be considered when applying coatings in areas where airborne overspray could damage automobiles, boats, and structures nearby. Heavy winds result in considerable loss of coating and in excessive drying of the droplets reaching the surfaee: This results in an inability of the film to flow together and create a continuous barrier free of "holidays." Such condi- tions can also create excessive amounts ofdry spray that can interfere with adhesion of the applied or subsequent coats. These problems can be avoided by utilizing brush or roller application methods instead of spray, or scheduling the work at the less windy times of day, changing materials to the dry-fog types that do not adhere or damage adjacent prop erty, scheduling the work so that if dry spray becomes attached to adjacent components it will not create a quality problem because it is attached to the final coat. 9. Coating Application 9.1 Residual Contaminants--Visually inspect the surface immediately prior to painting to ensure that spent abrasive, dust, and debris have been completely removed. Dust removal shall be considered satisfactory when the path left by a gloved hand wiped over the surface is barely discernible when viewed from a distance of 3 ft (l m). During this inspection, also ensure that any oil or grease contamination that may have become deposited on the surface is completely removed. This is accomplished by solvent cleaning in accordance with SSPC-SP1. 9.2 Quality Assurance--The inspector must ensure that: (1) coatings received at the fabricators or in the field meet the description of the products acceptable under the require ments of the specification; (2) they are properly mixed and thinned (where allowed); (3) colors match a visual standard provided that proper precautions have been taken to prevent damage to adjacent areas from cleaning and painting opera tions; (4) working practices are so scheduled that damage to newly applied coating is minimized; (5) application equip ment (brushes, spray) is acceptable for type, cleanliness, and usability; (6) weather conditions are acceptable under the requirements of the specification; (7) field-testing equipment on hand is in satisfactory working order ready for use; and (8) only the methods of application permitted under the specification are used and that their use is in accordance with 9.2.1 and 9.3 through 9.7. SSPC-PA1 is a specification for application of coating. 9.2.1 Film Defects--All coats should have nearly smooth, streamlined surfaces relatively free of dryspray, overspray, orange peel, fish eyes, pinholes, craters, bubbles, or other significant defects. Show through, insufficient hiding skips, and misses are not acceptable. Runs and sags should be brushed out during application. Abrasive, dirt, or other debris that becomes embedded in the paint film should be removed prior to the application of subsequent coats. 9.3 Brush Application--Painting by brush must be done in a neat, workmanlike manner to produce a smooth coat as uniform in thickness as possible. Coating should be worked into all irregularities in the surface, crevices, and comers. Runs, sags, or curtains should be brushed out. Surfaces that are inaccessible for painting with brushes and on which spraying is not permitted should have coating applied by means of sheepskin daubers. To provide adequate film thickness on places prone to premature breakdown, it is recommended that edges and comers ofall metal work, rivet heads, bolts and nuts, and all individual members, bars, shapes, and plates should be striped by brush painting in advance of the application ofcoating to other parts. 9.3.1 Brashes must be ofgood quality with pliable bristles. They should not exceed 4 in. (100 mm) in width and the 453 DUP0502 97634 D 3276 bristle length should be no less than 3'/2 in. (90 mm). When not in use, the brushes should be kept in a clean, acceptable condition. The inspector may prohibit the use of any brush not in an acceptable condition. 9.4 Spray Application--Spray application may or may not be allowed. Often it is acceptable in fabricating shops but, because of the possibility of damaging surrounding property or coating films from overspray, it may not be permitted in the field. The inspector should be familiar with the different kinds of spraying, which are compressed air spray, airless spray, hot spray, and hot airless spray. 9.4.1 The equipment should be suitable for the intended purpose, capable of properly atomizing the coating to be applied, and be equipped with suitable pressure regulators and gages. The equipment must be kept in a suitably clean condition to permit proper coating application without depositing dirt, dried coating, and other foreign materials in the film. The air supply for conventional and hot spray application should be free of moisture or oil. Airless spray equipment should be properly grounded. Any solvents left in the equipment should be completely removed before ap plying coating to the surface being painted. 9.4.2 Coating ingredients must be kept properly mixed in spray pots or containers during coating application, either by continuous mechanical agitation or by intermittent agita tion. Coating should be applied in a uniform layer, with overlapping at the edge of the spray pattern. The spray pattern should be adjusted so that the coating is deposited uniformly. During application the gun should be held at right angles (perpendicular) to the surface (not arced or fanned) and at a distance that will ensure that a wet layer of coating is deposited on the surface. The trigger of the gun should be released at the end of each stroke. Poor spray technique resulting in excessive overspray (or sand-like finish) should not be tolerated. All runs, sags, or curtains must be brushed out immediately or the coating will have to be removed and these areas repainted. 9.4.3 Usually brush striping of edges and other vulnerable locations as described in 9.3 is required. Brush or sheepskin daubers are used to coat all areas inaccessible to the spray gun and brushes and are used to work coating into cracks, crevices, and blind spots not adequately spray painted. 9.4.4 Particular care should be observed with respect to type and amount of thinner, coating temperature, and operating techniques in order to avoid depositing coating that is too viscous, too dry, or too thin when it reaches the surface. 9.5 Roller Application--Rollers that are clean and of a material not soluble in the coating to be applied should be used. Rolle- 'overs are available in a variety of diameters, lengths, typ of fabric, and fiber lengths. The nap (length) used on metal surfaces generally varies from l/t to % in. (25 to 75 mm). The longer fibers hold more coating but do not provide as smooth a finish. Therefore their use is generally restricted to rougher surfaces and faster drying coatings. There are also specialized rollers available for use on pipes, fences, and even pressure rollers that continually feed the coating to the roller cover. 9.5.1 The roller cover should be dipped into the coating until it is saturated and then rolled along the tray ramp until the coating is completely wetted in. The first load of coating on the roller should be applied to scrap material to force. AdditU air bubbles trapped in the nap. Proper roller techniq111 * ',0.1 v requires application in the form of a V or W depending U the size of the area involved. The coating should then ( ? cross-rolled to fill in the square created by the boundaries f the initial application. Only moderate pressure should k! used as heavy pressure can cause foaming and possib? aCes thai wents. *V2 Sh. cratering by entrapped air. Application should be finish^ with light perpendicular strokes in one direction (usual]! vertical) to provide the smoothest, most uniform finish. 1 9.6 Miscellaneous Methods--Methods such as mitts, and squeegees or trowels are used for special^ products or in situations where the conventional methods are not suitable due to the location or configuration of the work. 9.6.1 Painter's pads generally consist of a roller-type synthetic fabric attached to a foam pad. The size is generally 4 by 7 in. (100 by 175 mm) and the fiber length is 3/i in. (5 mm). Application technique with a pad on large surface areas is similar to that used with a roller. 9.6.2 Painter's mitts are lamb skin gloves that are dipped into the coating and are rubbed across the surface. They are ideal for application of coatings to odd-shaped surfaces such as pipes and railings. should 1 each co. accepter Except ^elding in the coticrct 1 contrac 9.6.3 Squeegee or trowel application is generally used for heavy-bodied thick-film coatings that cannot be applied by spray. 9.7 Rate of Application--Properly written specifications require certain minimum and maximum dry-film thick I from b concre \ withot ! 10.4 contin nesses for each coat. The requirements should be augmented with wet-film thickness figures calculated from the composi tion of the coating so that the proper dry-film thickness is obtained. (Equation shown in 7.3.3.2.) Wet-film thickness figures are useful to the inspector since he can often check as the work progresses to determine reasonably well that the desired amount of coating is being applied. Later, when the films are dry, the inspector should make spot checks with a dry-film measuring gage to ascertain acceptability of the coatings. Film thickness measurements are more informative than visual inspection, which may show only obvious nonuniform application. Instruments for measuring film thickness and the procedures for their use are described in 6.2.5 and 6.2.6. Nondestructive dry-film thickness gages and measurements are applicable to metal substrates only. 9.7.1 Thickness or coverage requirements apply to the whole structure, not some specific part. It is important that the painting inspector check all areas and determine the film thickness for each coat. For instance, if the "shop coat" requires a minimum of2 mils (50 pm) dry film, the inspector should ensure that it is obtained within the tolerances permitted in SSPC-PA2. The areas tested should be identi fied and recorded so that the dry thickness of added coating can be also determined. With nondestructive measuring instruments a 50-ft (15-m) long and 6-fit (1.8-m) high I-beam can be tested in 30 min and low areas if any, properly marked and recorded in the inspector's book. Because the shop prime coat inspector may not be the person doing the field coat application inspection, it is very important to record test results and send a copy to the field inspector in order to better determine thicknesses of subsequently applied coats. 1 DUP0502 97635 >rce out' ;hniqUe ding on then be lanes of auld be possible finished (usually ish. ; pads, cialized nethods i of the ler-type snerally is in. (5 surface dipped hey are :es such lsed for >lied by ications t thickmented >mposi<ness is tickness heck as hat the hen the ; with a of the anative avious ; film led in is and :o the int that die film p coat" ispector erances identicoating asuring I-beam iroperly use the ling the tant to ector in applied D 3276 |H, Additional Considerations [0.1 Ventilation--It is essential when painting in enclosed ^ces that adequate ventilation is provided for removal of Svents. [0.2 Shopcoat Repair--Normally after erection work, as riveting, bolting, welding, straightening, etc., has completed satisfactorily, areas of the shopcoat will be jjund to have been damaged. Damaged or bare areas must jjg thoroughly cleaned, prepared, and covered with one new Joat of shop or field primer. In addition, crevices and small jcks should be thoroughly cleaned and spot-primed. After jjying, the crevices and cracks should be filled with an jjceptable caulking compound as required by the specificajon. The specified field coats should then be applied over the jjtire structure. [0.3 Painting Schedule--As`indicated in 5.4.4, painting jjjould proceed by sections, bays, or parts of the work, and jach coat on each section should be applied entirely and accepted by the inspector before a succeeding coat is applied. Except for any shop coat touch ups made necessary by ^elding, etc., none of the metal that will be exposed to view jii the completed structure is to be field-painted until all concrete has been placed. Care must be taken by the contractor during painting operations to protect concrete [com being stained by the coating being applied. Any stained concrete surface must be restored to its intended color without damage to the concrete. [0.4 Film Integrity--Each coat should be applied as a continuous film of uniform thickness, free of holidays and pores. Any thin spots or areas missed in the application should be repainted and permitted to dry before the next coat is applied. 10.5 Recoat Time--Each coat must be dried throughout the full thickness of the film before application of the succeeding coat. Coating is considered dry for recoating when the next coat can be applied without the development of any detrimental film irregularities such as wrinkling, lifting, or loss of adhesion of the previous coat. For most coatings the time to dry for recoat, even under optimum conditions varies with their composition and that of the subsequent coat. Thus, an oil-based coating may take 2 to 4 days to harden sufficiently to be overcoated with a coating of the same type. However, it may take 3 or 4 months to harden to be satisfactorily overcoated with a vinyl coating or other type of coating containing strong solvents. The coating manufacturer's literature should be consulted for recoat times. 10.6 Coating System Failure--Failure of completed coating work may be the result of several factors. Most obvious is noncompliance with the specifications indicating insufficient inspection of surface preparation, coating quality, coating application, or conditions during application and drying/curing. On the other hand, failure may be due to improper specification of coatings for the intended use. Defective coatings should be removed in their entirety, the surface recleaned, and the specified coatings, or their alterna tives, applied. 455 DUPO 502 97636 D 3276 APPENDIX ! \ Nonmandatory Information XI. INSPECTION CHECKLIST I Xl.l The checklist in Fig. XI. 1 lists the key elements to be used for inspection of industrial coating work. Many of the details covered may be in a specification for a particular project. A job specification for painting should include the I coatings to be used. The various items are explained in detaj] I in the text of this guide. TASK I Surface Condition Examination 1 Condition of edges, weld splatter 2 Grease or oil, or both 3 Chalk, mildew 4 Protective coverings in place 5 Air temperature 6 Surface temperature 7 Wind direcUon, velocity 8 Dew Point, RH 9 Visible moisture I Surface Condition: 1 Visual observation and touch 2 Visual observation and clean white rag 3 Visual observation and magnifying glass 4 Visual observation 5 Air thermometer 6 Surface thermometer ^ 7 Current weather report 8 Sling psychrometer 9 Direct observation I Cleanliness--Many materials if not re. moved from the surface will affect the life of the coating. These include oil, grease soil, weld spatter and slag which make it impossible to obtain proper adhesion to the metal surface (5.2.1, 5.4). Careful observation is the key to making certain that a sound surface is- available fcr painting. Factors are listed which win affect job Quality (9.1). >ASK- V Coating 1 Tim appl 2 Coa 3 Con 4 Prot 5 Tim 6 Sun 7 Co d and 8 Cor cedi 9 Ind' 10 Pro 11 File --V II Safety on the Job: Protective clothing Respirator Safety glasses Ear protection II Safety on the Job: OSHA Hazard Communication Standard Product MSD sheets Municipal and state regulations II There are a number of hazards associated with any painting operation; safety regula. tions must be observed and unsafe conditions or practices should be reported promptly to management (1.2, 5.3). ! i i Ill Blast Cleaning: 1 Type and size abrasive 2 Clean and dry abrasive 3 Recycled abrasive test 4 Compressed air check 5 Nozzle air pressure IV Surface Preparation: 1 Dust and abrasive removal 2 Degree of cleanliness 3 Profile measurement 4 Magnetic base reading III Blast Cleaning: 1 Sieve analysis and visual observation 2 Visual observation 3 Water test 4 White blotter 5 Pressure gage III Blast cleaning is used to remove foreign materials from a metal surface and to provide a roughened surface by means of a dry sand, grit, or shot blast impinging the surface with hard abrasive particles impelled by air (5.3.4). The minimum and maximum particle size of the abrasive are specified as a means of controlling the surface profile. Precautions must be taken that blasting equipment is operated properly (5.2.3). : ! ! I IV Surface Preparation: 1 Visual observation 2 Pictorial Standard D2200 should be used by the inspector on ajob involving painting of structural steel to determine whether the degree of surface prepara tion specified in a contract has been attained by the contractor (5.1.1). 3 Keane-Tator comparator for visual comparisons of the profile against a reference disk for sand, grit, and shotblast-cleaned steel (6.1.1). Testex Press-O-Film tape is used to create an exact replica of the profile on a special material. The tape is measured in the field using a spring micrometer to determine average maximum profile height. 4 Magnetic thickness gage (6.2.6) IV Surface preparation is one of the most important factors affecting the perform ance ofpaint. The specifier will determine I the proper level according to the expected | service life of the structure and type of i paint specified (5.1). Surface Profile--The texture of the metal surface has a signifi cant effect on the performance of coatings since it increases the surface area to which the coating can develop adhesion. 12 Re 13 Im 14 Fil VI Recor, 1 Ret Bat O 2 Re 1,1 FIG. Xl.l Inspection Checklist 456 DU PO50297637 D 3276 elude the l in detail if not re fect the life ail, grease, ;h make it dhesion to ). Carefhl ing certain nlable for vhich will associated fety regulasafe condi: reported 5.3). we foreign ce and to > means of impinging e particles n particle ified as a ce profile, at blasting (5.2.3). ' the most performletermine : expected d type of :file--The a signifif coatings i to which jn. y Coatings Application: 1 Time from surface preparation to application 2 Coating viscosity 3 Compressed air check 4 Protective coverings in place 5 Time application began 6 Surrounding air cleanliness 7 Continue to monitor temperature and humidity conditions 8 Correct coating and mixing pro cedure 9 Induction time observed 10 Proper percent agitation 11 Film thickness --Wet --Dry 12 Recoat Times Observed 13 Intercoat Cleanliness 14 Film Delects, Voids, etc. VI Recordkeeping: 1 Record all details Applicator Manufacturer Batch #'s Container Condition 2 Record Observations from Sections I, in, IV, and V of Fig. XI. I V Coatings Application: 1 Record 2 Dip-type viscosity cup D 4212 3 White blotter 4 Visual observation 5 Record 6 Visual observation 7 Visual observation 8 Record coatings batch numbers mix ing procedure 9 Visual observation 10 Visual observation 11 Film thickness gages V Many factors are important in ensuring proper application ofcoatings. The details are covered in this guide (Section 9). In particular, note: Dry-film thickness mea surements are of great importance be cause the protection of the substrate is directly related to the thickness of the coating. There are two ways of making the measurements, nondestructively or de structively (6.2.5). Wet (Notched Gage)--This device has a senes of calibrated steps for mea suring thin to heavy coats. The true wet-film thickness lies between the highest step coated and the next highest that was not coated. This method is not as accurate as the interchemical gage. Interchemical Gage--This type of in strument is designed to measure the thickness of a wet film of paint. Nondestructive Film Thickness Gages are widely used for field and shop inspection. For ferrous metals they are based on magnetism, and for nonmagnetic metals, inductance and eddy currents. See guide for discussion of types. Dry (Tooke Gage)--The Tooke paint inspection gage is designed to measure paint film thickness by microscopic observation of a cut into the paint film. 12 Record time application completed 13 Tape test D 3359 14 Holiday detector VI Recordkeeping: Inspector's log book VI Maintenance ofa record book containing all transactions between the inspector and the contractor is essential to eliminate contract disputes. Details of the many steps involved in proper coatings applica tion must be recorded (Section 4). FIG. XI.1 Inspection Checklist (continued) The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by tha responsible technical committee and must be reviewed every live years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will rscehie careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050297638 Designation: D 3281 - 84 (Reapproved 1989) Standard Test Method for Formability of Attached Organic Coatings with Impact-Wedge Bend Apparatus1 This standard is issued under the fixed designation D 3281; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in-parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 6.5 Pre 180) ant 'he wed; tipact re 6.6 Af jspect v fid adhi rogressi 6.7 M dge of i >ast sev. 1. Scope 1.1 This test method describes a method of evaluating the formability of organic coatings intended for application to strip metal substrates by coil-coating or other factory appli cation methods. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Significance and Use 2.1 This test method is designed to provide a uniform procedure for determining the degree of flexibility and adhesion of factory-applied organic coatings on strip metal'. 2.2 It should be recognized that some metal substrates will crack during forming and that the organic coating may crack accordingly. purchaser and the seller. Prior to application of the coating, N./' .edges of the specimens that will be bent in the test shall be rounded slightly to remove burrs in order to eliminate effects 6.8 D dhesivc associated with cracking of a sharp metallic edge when bent. ape in N,-' 1--When metal thickness exceeds 0.025 in. (0.64 mm), ending complete compression of the bend may not occur with a single impact. lian 11 4.2 The-coating under test shall be applied to the clean aost ex base metal after the agreed-to surface preparation of the a me metal substrate has been completed. The coating shall be tie ben applied to one or both sides of the metal (as specified) in a 6.9 1 manner that'will provide a uniform coating thickness. The ilm rei dry film thickness shall not vary more than 0.1 mil (2.5 his rat pm) from the specified thickness agreed upon between the purchaser and the seller. The method ofapplication, the cure Pre of the film, the time between the application of the coating 7.1 and the testing of the specimen, as well as the temperature . netho and humidity environment used for aging the film during neasu this period, shall be agreed upon between the purchaser and ; idhesi the seller. atorif 3. Apparatus 3.1 Impact-Type Wedge Bend, assembly illustrated in Fig, l.2 The instrument contains a 4-lb (1.82-kg) impacter rod with one flat end that slides in a vertical slotted guide and serves as a falling weight to hammer the wedge mandrel with the flat end. A knurled cover inserted in the wedge mandrel impact test hole serves as the impact point. When positioned properly the lifting knob on the impacter coincides with the zero mark on the guide tube. The spacer block is removed from the front edge of the wedge mandrel so that the taper is 0 to Vs in. (0 to 3.2 mm) front to back. 3.2 Cellulose Adhesive Tape, V* in. (20 mm) wide. 4. Test Specimens 4.1 Suitable substrates for the test specimen (including, thickness) shall be employed and agreed upon between the purchaser and the seller (Note 1). The dimensions ofthe base metal panel shall be 4 in. (100 mm) in width, with a maximum length of 12 in. (300 mm). The surface prepara tion of the base metal shall be agreed upon between the 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.53 on Coil Coaled Metal. Current edition approved April 27. 1984. Published December 1984. Originally published as D 3281 - 73. Last previous edition D 3281 - 73 (1979). 2 The Gardner Coverall Impact Tester available from BYK-Gardner, Inc. Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910, has been found satisfactory for this purpose. Use of other equipment should be agreed upon by the purchaser and seller. S. Conditioning and Number of Tests 5.1 Test at least three replicate specimens under the conditions of temperature and humidity mutually agreed w upon between the purchaser and the seller. Unless otherwise Be specified by the purchaser and the seller, make measure ilaser ments at 73.5 3.5"F (23 2`C) and 50 5 % relative ihoul humidity after equilibrating at these conditions for at least 24 :onfi h. 6. Procedure 6.1 Place the specimen, coated side down, under the Vs-in. (3.2-mm) cylindrical mandrel. Slide the specimen to the rear of the mandrel platform until the edge is flush with the two studs located at the rear of the platform. N,-' 2--Since the test is usually more severe if the panel is bent parallel to the original rolling direction of the base metal, the direction of the bend'with respect to the "grain"' of the; base metal should be agreed uppn between the purchaser and the sellerfand reported. 6.2 Raise the remainder of the panel at a uniform velocity to bend the specimen 170 to 180in a time not to exceed 5 s. 6.3 Slide the spacer located under the impact platform to the extreme front ofthe tester and tighten it in place with the adjustment screws provided. This allows the impact platform to create a wedge that provides stress angles between 170 and 180. N01' 3--The end of the specimen with the 180 stress angle is defined as having a zero T (0T) bend. 6.4 Center the bent specimen under the impact platform. Place the longest segment of the specimen downward. 458 DU PO50297639 iting, ill be Sects bent. mm), 'pact. Sean f the 11 be in a The 2.5 i the cure ating iture tring and the ;reed wise sureative st 24 rear two bent ion of .greed ocity i 5 s. m to hthe form ) and gle is orm. D 3281 , 5 predetermine the load required to result in a OT bend ' -- J run all tests using the same substrate at this load. >ue wedge bend required shall be obtained with a single ' pact representing the minimum force to obtain a OT bend. '^6 After impact, remove the specimen and visually , Jjct without magnification the bent portion for cracking adhesion loss, starting at the most severe bend and pressing outward. Q ^7 Measure the distance fractured (cracking) from the ,,,e of the most severe bend outward to the edge with the least severe bend in inches or millimetres. <|23{ 4--Disregard heavy beads of coadng on the edges. ( g Determine film adhesion loss by firmly applying the ^Ijesive tape to the entire bend area and then removing the (apg in a uniform rapid motion. The time between the first fading of the specimen and removal of tape shall not be less ^3 l nor more than 5 min. Start removal from the edge of most extreme bending (OT edge) and remove the tape rapidly j0 a motion parallel to the surface ofthe longitudinal edge of jbe bend, such that the tape is pulled back upon itself. 6,9 Examine the taped area and measure the amount of (ym removed. It should be noted that the primary concern of ibis rating is the maximum distance of adhesion failure. 7. precision 7.1 On the basis of an interlaboratory study of this test method in which two operators in each of five laboratories measured two replicates on two days for cracking and adhesion, the standard deviations within and between labo ratories were found to be as follows: Standard Deviation Cracking, Adhesion, mm mm Within laboratory Between laboratory 2.0 3.9 4.7 10.0 Based on these standard deviations, the following criteria should be used to judge the precision of results at the 95 % confidence level: FIG. 1 Coverall Impact Tester 7.1.1 Repeatability--Two measurements obtained by the same operator should be considered suspect if they differ by more than , Crackiug, mm Adhesion, mm 5.8 [1.4 7.1.2 Reproducibility--Two measurements, each the mean of duplicate measurements, obtained in different laboratories should be considered suspect if they differ by more than Cracking, mm Adhesion, mm 16.8 35.7 the American Society for Testing and Materials takes no position respecting the validity of any patent rights assertedin connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn: Your comments are invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 459 DUP050297640 Designation: D 3322 - $2 (Reapproved 1991) Standard Practice for Testing Primers and Primer Surfacers Over Preformed Metal1 Abrasi Air This standard b issued under the fixed designation D 3322; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. Fall Adhei Sci Pai 1. Scope 1.1 This practice covers the selection and use of proce dures for testing primers and primer surfacers. The test methods included are listed in Table 1. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents > 2.1 ASTM Standards: B 117 Method of Salt Spray (Fog) Testing2 D1186 Test Methods for Nondestructive Measurement <$ Dry Film Thickness of Nonmagnetic Coatings Applied; to a Ferrous Base5 D 1308 Test Method for Effect of Household Chemicab on Clear and Pigmented Organic Finishes5 D 1400 Test Method for Nondestructive Measurement ofj Dry Film Thickness of Nonconductive Coatings Ap. plied to a Nonferrous Metal Base5 D 1474 Test Methods for Indentation Hardness of Organic Coatings5 D 1640 Test Methods for Drying, Curing, or Film Forma. tion of Organic Coatings at Room Temperature5 D 1729 Practice for Visual Evaluation of Color Differences of Opaque Materials6 Ta Chert He De Hi Chip Colo Vi In Cra< Elor C C Filit Glo Hat Hoi Mil Ou C 540 Test Method for Image Gloss of Porcelain Enamel D1730 Practices for Preparation of Aluminum and Alu Surfaces3 minum-Alloy Surfaces for Painting7 D16 Terminology Relating to Paint, Varnish, Lacquer, D1731 Practices for Preparation of Hot-Dip Aluminum and Related Products4 D 522 Test Methods for Mandrel Bend Test of Attached Organic Coatingss D 523 Test Method for Specular Gloss5 Surfaces for Painting7 D 1732 Practices for Preparation of Magnesium Alloy Surfaces for Painting7 D1733 Method of Preparation of Aluminum Alloy Panels Pr Si Si w D 609 Practice for Preparation of Steel Panels for Testing for Testing Paint, Varnish, Lacquer, and Related Paint, Varnish, Lacquer, and Related Products5 Products8 D 610 Test Method for Evaluating Degree of Rusting on D1735 Practice for Testing Water Resistance of Coatings Painted Steel Surfaces5 Using Water Fog Apparatus5 D658 Test Method for Abrasion Resistance of Organic D1737 Test Method for Elongation of Attached Organic Coatings by Air Blast Abrasive5 Coatings with Cylindrical Mandrel Apparatus9 D 660 Test Method for Evaluating Degree of Checking of D 2091 Test Method for Print Resistance of Lacquers5 Exterior Paints5 D 2092 Practices for Preparation of Zinc-Coated (Galva* D 661 Test Method for Evaluating Degree of Cracking of nized) Steel Surfaces for Painting5 Exterior Paints5 D 714 Test Method for Evaluating Degree of Blistering of D 2197 Test Methods for Adhesion of Organic Coatings by Scrape Adhesion5 Paints5 D 823 Test Methods for Producing Films of Uniform D2201 Test Method for Preparation of Hot-Dipped Noupassivated Galvanized Steel Panels for Testing Paint, Thickness of Paint, Varnish, and Related Products on Test Panels5 D 870 Practice for Testing Water Resistance of Coatings Using Water Immersion5 D 968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive5 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers5 Varnish, Lacquer, and Related Products5 D 2244 Test Method for Calculation of Color Differences from InstrumentaUy Measured Color Coordinates5 D2246 Test Method for Finishes on Primed Metallic 3. Substrates for Humidity-Thermal Cycle Cracking5 D2248 Practice for Detergent Resistance of Organic J Finishes5 vs D2454 Practice for Determining the Effect of Overbakingg| on Organic Coatings5 |r D2803 Test Method for Filiform Corrosion Resistance off 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Organic Coatings on Metal5 Related Coatings and Materials and is the direct responsibility of Subcommittee DOl.55 on Factory-Applied Coatings on Preformed Products. D 3170 Test Method for Chipping Resistance of Coatings5 Current edition approved Nov. 26, 1982. Published January 1983. Originally published as D 3322 - 74. Last previous edition D 3322 - 74a. 2 Annual Book ofASTM Standards, Vols 03.02 and 06.01. 1 Annual Book ofASTM Standards, Vol 02.05. 4 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 3 Annual Book ofASTM Standards, Vol 06.01. 6 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 7 Annual Book ofASTM Standards, Vols 02.05 and 06.01. 8 Discontinued; see 1980 Annual Book ofASTM Standards, Part 27. 9 Discontinued; see 1988 Annual Book ofASTM Standards, Vol 06.01. 460 DU P050297641 # D 3322 cement 0f Appii^ Chemicals rement 0f stings Ap. Organic * Formare5 'ifferences and Alu- luminum im Alloy oy Panels Related Coatings 1 Organic luers5 1 (Galva- tings by d NonPaint, ..erences ites5 Metallic ng5 Organic erbaking stance of boatings5 TABLE 1 Test Methods Property Section Tbrasiai resistance: 0 blast abrasion tester Falling sand method Adhesion: Scrape adhesion Parallel-groove adhesion Tape adhesion chemical resistance: Household chemical resistance Detergent resistance Hydrocarbon resistance chip resistance minr difference: Visual evaluation instrumental evaluation cracking resistance Elongation: Conical mandrel Cylindrical mandrel Inform corrosion J0$$ Hardness Holdout Widew resistance Outdoor exposure: Blistering Cracking Rusting Checking Print resistance Sait spray resistance SancSng properties Water resistance: High humidity Water immersion Weldability 5.2 5.2 5.3.2 5.3.2 5.3.2 5.4.2 5.4.3 5.4.4 5.5 5.6 5.6 5.7 5.8 5.8 5.9 5.10 5.11 5.12 5.13 5.14.2 5.14.2 5.14.2 5.14.2 5.15 5.16 5.17 5.18.2 5.18.3 5.19 > u.s. Military Specification MIL-P-46105 (MR). ASTM Method Fed. Test Method Spec. No. 1418 D 658 D968 D 2197 D2197 D 3359 D1308 D2248 D3170 D 1729 D 2244 D 2246 D 522 D 1737 D 2803 D 523 D 1474 C540 D 714 D 661 D 610 D 660 D2091 B 117 D 1735 D 870 6191 6303.1 6302.1 6011 4249.1 6123 6101 8271.1 6461 6471 6451 6421 6061 6321 A D3359 Test Methods for Measuring Adhesion by Tape Test5 D3456 Practice for Determining by Exterior Exposure Tests the Susceptibility of Paint Films to Microbiolog ical Attack5 2.2 Federal Test Methods:10 141B/6011 Immersion Resistance 141B/6271.1 Mildew Resistance 141B/6321 Sanding Characteristics 2.3 U.S, Military Specification: MIL-P-4610510 3. Terminology 3.1 Definitions: 3.1.1 primer--the first of two or more coats of paint, varaish, or lacquer system (same as in Terminology D 16). 3.3.2 primer surfacer--a pigmented coating for filling minor irregularities which is sanded to obtain a smooth "inform surface preparatory to applying finish coats. A Primer surfacer is not usually applied over a primer. Significance and Use 4.1 Primers and primer surfacers may be used over many 7. : '"Available from Standardization Documents Order Desk, Bldg. 4 Section D, i.01. M Robbins Ave., Philadelphia, PA 19111-5094. different surfaces top coated with one or more of a variety of coatings and subjected to many kinds of wear and exposure. 4.2 The selection of the tests to be used for any given product or system must be governed by experience and by the requirement agreed upon between producer and user. 5. Panel Preparation 5.1 Treatment of Substrate--Preparation of test panels should include any cleaning treatment agreed upon between purchaser and seller or one of the following ASTM Practices: D 609, D 1730, D 1731, D 1732, D 1733 and D 2092, and Test Method D 2201. 5.2 Substrate, Film Thickness and Application Means-- Conduct performance tests on the specified substrate on coatings having a film thickness agreed upon between the purchaser and seller. Primers are generally applied to a dry film thickness of 0.3 to 1.5 mils (8 to 38 pm) and primer surfacers to film thickness of 0.7 to 2.0 mils (17 to 50 pm). Unless otherwise agreed upon, apply primers and primer surfacers in accordance with Test Method D 823. 5.3 Measurement ofFilm Thickness--Since the properties of the primer or primer surfacer can vary considerably with the thickness of the coating, it is important to know the film thickness. Measure the film thickness in accordance with Test Methods D 1400, D 1005, or D 1186. 5.4 Drying ofPrimer or Primer Surfacer: 5.4. i Before tests are rum air dry or bake the primer or primer surfacer according to the schedule and temperature and age as agreed upon between the purchaser and seller. 5.4.2 Overbake the primer or primer surfacer to deter mine the time/temperature effect on the physical and chem ical properties. Do this in accordance with Practice D 2454. 5.4.3 It may be desirable for some reason (handling, stacking, etc) to determine the various stages and rates of film formation in the drying or curing of primers and primer surfacers at room temperatures. Do this as described in Test Method D 1640. 6. Physical Properties of The Dry Film 6.1 Primers and primer surfacers are usually (but not always) topcoated. Therefore, many of the following tests should be run on the complete system (substrate/primer or primer surfacer/topcoat). Some of the tests however are for the untopcoated primer or primer surfacer. The properties required of a primer or primer surfacer depend on the intended end use and the tests to be used should be selected on the basis of experience and agreed upon between the purchaser and seller. 6.2 Abrasion Resistance--Determine the abrasion resis tance as described in either Test Method D 658 or D 968. 6.3 Adhesion: 6.3.1 The primer or primer surfacer of a specified sub strate as agreed upon by the purchaser and seller is subjected to an adhesion test to determine the degree of attachment the coating has to the substrate. 6.3.2 Determine the adhesion of the primer or primer surfacer as described either in Test Methods D2197 or D3359. 6.3.3 The above methods* in addition to measuring the adhesion of the. coating to the substrate, can also be used to determine the intercoat adhesion between the topcoat and 461 DUP050297642 D 3322 the primer or primer surfacer. agreed upon by the purchaser and seller. Other methods of th< 6.4 Chemical Resistance: determining hardness may be used as agreed between pnr. 6.4.1 Coating systems frequently come into contact with chaser and seller. de various chemicals that may have an effect on the properties 6.12 Holdout--Holdout is the ability of a primer or sa; I of the system. Failure when it occurs is usually in the form of discoloration, change in gloss, blistering, softening, swelling, dissolving, or loss of adhesion. Unless a primer is to be left primer surfacer to give a smooth (nonporous), uniform appearance when topcoated. This property can be evaluated visually or by instrumental means. One method of mea in' up untopcoated in actual service, primers and primer surfacers suring for holdout is described in Test Method C 540. should be topcoated with the appropriate product before undergoing chemical resistance tests. 6.4.2 Household Chemical Resistance--Determine the 6.13 Mildew Resistance--Test mildew resistance in accor dance with Method 6271 of U.S. Federal Test Method Standard No. 14IB or Practice D 3456. de hi effect of chemicals in accordance with Test Method D 1308. 6.14 Outdoor Exposure: us 6.4.3 Detergent Resistance--Determine the resistance to 6.14.1 Primers and primer surfacers can have an impor- failure under conditions ofimmersion in a detergent solution tant effect on the durability of any paint system destined for in accordance with Practice D 2248. exterior use. While the accelerated tests given in other 6.4.4 Hydrocarbon Resistance--Test hydrocarbon resis sections ofthis recommended practice are intended to enable tance in accordance with Method 6011 of U.S. Federal Test one to predict performance, actual outdoor exposure should Method Standard No. 141B. be made. Usage of paint systems is so varied that no one set ! 6.5 Chip Resistance--The chip resistance of a primer or of conditions (length of exposure or place of exposure) can primer surfacer is the ability of a film to withstand sudden be given in this practice to cover all situations. These impact from stones, gravel, etc, without being loosened from conditions as well as the type of substrate, substrate prepara the substrate. Determine chip resistance by Test Method tion, etc should be agreed upon between the purchaser and D 3170. the seller. However, it is suggested that, unless otherwise 6.6 Color Difference-Pigmented Dry Film--The color dif agreed upon, prepare panels for outdoor exposure in accor* I ferences between two similarly homogeneously colored, dance with Section 4 of this practice. opaque film such as those formed by primers or primer 6.14.2 Many properties of organic coating systems should j surfacers may be determined using visual evaluating tech be evaluated periodically throughout the outdoor exposure 1 niques or by instrumental means. Determine color differ period. Where failures occur on a topcoated system, expert f ences visually using Practice D 1729. Determine color differ ence is required to determine whether or not the primer or J ences instrumentally using Test Method D 2244. primer surfacer is involved. Properties most likely to involve | j 6.7 Cracking Resistance--A test for resistance to temper the primer or primer surfacer may be evaluated as follows; 1 ature and humidity changes, or a cold cracking test as it is Blistering, Test Method D714; Cracking, Test Method : sometimes called, is designed to give an indication of the D 661; Rusting, Test Method D 610; Checking, Test Method- resistance of a coating system to cracking or checking caused D 660. i by temperature and humidity changes and also by aging. The 6.15 Print Resistance--A print test can be used to deter degree of correlation between accelerated crack results and mine the degree of thermoplasticity or solvent retention ofa ;j long term room temperature aging varies with the types of film and hence whether the product can be safely stacked or 3 coating. The industry uses the test widely and it is felt that a packaged and, in the case of a thermoplastic film, at what system showing good cold crack resistance will perform temperature the film prints or mars. A print test can also be satisfactorily in service. Some factors that can affect results used to determine the degree of marring due to pressure, j are type of substrate, substrate thickness, primer, primer Determine the imprinting and thermoplasticity of primer or >; ! surfacer, topcoat, and film thickness of the different coatings. primer surfacer films as described in Test Method D 2091 1 I Determine cracking resistance in accordance with Test Method D 2246. 6.8 Elongation--An elongation test may be used as an is 6.16 Salt helpful in SdeptrearymRineisnisgtathnceeir--reSsaislttasnpcreaytotefsatiilnugreoifncosaetirnvgiscle^ under conditions of high humidity and salt concentrations. |T indication of the flexibility of an attached primer or primer Under accelerated conditions of laboratory testing the surfacer. It can also show whether there is any change during perature, the pH, the concentration of the salt solution andf' aging. Determine elongation by Test Methods D522 or other physical properties can be controlled. The selection of| D 1737. the substrate, the application technique, the choice of 6.9 Filiform Corrosion Resistance--Filiform corrosion is topcoat, the manner in which the coating is scribed, tE| a type of corrosion that occurs under coatings on metal location or position of the panels within the cabinet, m substrates and is characterized by a definite thread-like length of the test, the inspection of panels and the method: structure and directional growth. Determine the suscepti reporting results must be agreed upon between the pure! bility of organic films over metal substrates to this type of and seller. Test for salt spray resistance in accordance wiri corrosion by Test Method D 2803. 6.10 Gloss--Determine the gloss of primers and primer Method B 117. 6.17 Sanding Properties: surfacers in accordance with Test Method D 523. 6.17.1 Sanding properties are normally expectedjj| 6.11 Hardness--Determine the film hardness of primers primer surfacers only. Method 6321 of U.S. Federal and primer surfacers in accordance with Test Methods Method Standard No. 14IB covers this property. D 1474, using either Test Method A (Knoop indentation 6.17.2 Prepare and dry a film of the material to be test! hardness) or Method B (Pfund indentation hardness) as as specified in the product specification. Scuff the surface d! 462 DUP0502 97643 D 3322 Lethods of veen Pur. 'rimer 0r unif0nt) evaluate Lf niea' >40. ` accor; Method m il:npor. stined f0r in other to enable ire should io one set sure) can 's* These 5 preparahaser and otherwise in accor- 1 dried film manually with 400 softback sandpaper. p jjjjine the film for gouging and deep scratches and f^rtiiine whether there has been .any clogging of the ^dpaper. Depending on the end use of the primer surfacer Solved, other methods of sanding may be used as agreed 'non by the purchaser and seller. g_l8 Water Resistance: 18.1 Testing of coating systems with water is helpful in determining their resistance to failure under conditions of ^ humidity or water immersion. Failure in water tests is j ^jjally evidenced by blistering, dulling, softening or loss of adhesion which does not disappear or recover upon evapora tion of the absorbed water. 6.18.2 Determine the resistance to failure under condi tions of high humidity in accordance with Practice D 1735. 6.18.3 Determine the resistance to failure under condi tions of water immersion in accordance with Practice D 870. This test is best suited for coating systems that will actually be soaked in water during service. 6.19 Weldability--In some instances it is necessary to weld metal that has been primed. The welding characteristics of a primer or primer surfacer may be tested in accordance with U.S. Military Specification MIL-P-46105 (MR), Section 4.4.11. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised thet determination of the validity of any such patent rights, and the risk of infringemem of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not revised, either reapprovedor withdrawn. Yourcomments are invited eitherforrevision of this standard or for additionalstandards and should be addressee/ to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel thet.your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ns should exposure n, experiprimer or o involve s follows: Method t Method to deterltion of a tacked or , at what n also be pressure, rimer or ) 2091. coatings n service itrations. the temltion and lection of ce of the ibed, the >inet, the lethod of purchaser mce with 9 ected of eral Test be tested ;urface of 463 DU P050297644 Designation: D 3323 - 80 (Reapproved 1988),'ei An American National Sts Standard Guide for Testing Inferior Solvent-Reducible Flat Wall Paints1 This standard is issued under the fixed designation D 3323; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval, A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. " N45' --Editorial changes were made throughout, including the title, in October 1988. 1. Scope 1.1 This guide covers the selection and use of procedures for testing interior solvent-reducible flat wall paints, such as alkyd or other solvent-thinned finishes. The test methods included are listed , in Tables 1 and 2. All of these test methods may not be required for each paint. Selection of the test methods must be governed by experience and the requirements in each individual case, together with agree ment between the purchaser and seller. 1.2 This guide covers the testing of ready-mixed finish coats for application by brushing, roller coating, spraying, or other methods, on wood, plaster, wallboard, masonry, previ ously painted surfaces, and other interior architectural sur faces. 2. Referenced Documents 2.1 ASTM Standards: D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester3 D154 Guide for Testing Varnishes4 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints5 D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts4 D 522 Test Methods for Mandrel Bend Test of Attached Coatings4 D 523 Test Method for Specular Gloss4 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer4 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels4 D1208 Test Methods for Common Properties of Certain Pigments6 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and is the direct responsibility of Subcommittee D01.42 on Architectural Finishes. Current edition approved Oct. 31, 5980. Published December 1980. Originally published as D 3323 - 74. Last previous edition D 3323 - 79. 2 Annual Book ofASTM Standards, Vols 06.01, 06.02 and 06.03. 3 Annual Book ofASTM Standards, Vols 05.01, 06.01, and 06.03. 4 Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 6 Annual Book ofASTM Standards, Vol 06.02. D1210 Test Method for Fineness of Dispersion of Pig, ment-Vehide Systems4 D1310 Test Method for Flash Point and Fire Point Liquids by Tag Open-Cup Apparatus7 D1475 Test Method for Density of Paint, Varnish, La>J quer, and Related Products4 D1554 Definitions of Terms Relating to Wood-Base FibeJ and Particle Panel Materials8 D1640 Test Methods for Drying, Curing, or Film Form! tion of Organic Coatings at Room Temperature4 D1729 Practice for Visual Evaluation ofColor Differed,, of Opaque Materials9 II D1737 Test Method for Elongation of Attached Organf Coatings with Cylindrical Mandrel Apparatus10 D2196 Test Methods for Rheological Properties of Nod| Newtonian Materials by Rotational (Brookfield) Vi' cometer4 D2197 Test Methods for Adhesion of Organic Coatings by| Scrape Adhesion4 | D2244 Test Method for Calculation of Color Difference! From Instrumentally Measured Color Coordinates4 ,|g D2369 Test Method for Volatile Content of Coatings4 D2371 Test Method for Pigment Content of Solvent^ Redudble Paints4 D2372 Method of Separation of Vehicle from Solvent- Reducible Paints4 D 2486 Test Method for Scrub Resistance oflnterior Later Flat Wall Paints4 D2621 Test Method for Infrared Identification of Vehicle) Solids from Solvent-Reducible Paints4 D2801 Test Method for Leveling Characteristics of Paints| by Draw-Down Method11 ;J D2805 Test Method for Hiding Power of Paints by Reflectometry4 D3278 Test Methods for Flash Point of Liquids by;| Setaflash Closed-Cup Apparatus7 f E 105 Recommended Practice for Probability Sampling o| Materials9 E 313 Test Method for Indexes of Whiteness and Yellow^ ness of Near-White Opaque Materials9 7 Annual Book ofASTM Standards, Vol 06.03. 8 Annual Book ofASTM Standards, Vol 04.09. 8 Annual Book ofASTM Standards, Vol 14.02. 10 Discontinued; see 1988 Annual Book ofASTM Standards, Vol 06.01. 11 Discontinued; see 1989 Annual Book ofASTM Standards, Vol 06.01. 464 DUP050297645 # D3323 5 TABLE 1 List of Test Methods by Properties Test Method Section ASTM Test Method Federal Test Method Std. No. 141 Ke lt of ; Lac- -iber rma- Jnces ?anic NonVis- gsby Sampling Liquid paint properties: Absorption Coarse particles and foreign matter Color acceptance Condition in container Consistency Fineness of dispersion Flash point Rheological properties of non-Newtonian materials Skinning Weight per gallon Paint application and film formation: Application of brushed films Application of sprayed films Drying time Leveling properties Producing films of uniform thickness Boiler coating properties Working properties Appearance of dry paint film: Color difference by visual comparison Color difference by instrument evaluation Specular gloss (sheen) Properties of dry paint film: Adhesion Cleanability Scrub resistance Washability Elongation Fume resistance Yellowness index Hiding power (dry opacity) Analysis of paint: Identification of vehicle solids Pigment content Separation of vehicle Volatile content Water content 5 6.10 6.3 6.8 6.2 6.6 6.4 6.7 6.9 6.1 6.5 7.1 7.2 7.3 7.4 7.5 7.6 7.7 8.1 8.2 8.3 9.1 9.2 9.2.1 9.2.2 9.3 9.4 9.5 8.4 10.1 10.6 10.4 10.5 10.2 10.3 E 105 0185 0 562 01210 D 1310, D 93, D 3278 D2196 D 154 D 1475 0 1640 D 2801 O 823 D 1729 D 2244 D 523 D 2197 D 2486 D 2486 D1737, D 522 E 313 D 2805,D 344 D 2621 0 2371. D 2372 D 2369 D1208 1022 4421 4091T 3011 42811 441 If 3021 4184f 2141, 4321 2131,4331 4061 2162 4335 4541 4249f 6123t 6103f 6303T 6141 6221 6131 4021, 4022f 4032f 4041f, 4042 4081 2aces 4 )S4 ventiventLatex :hicle faints .ts by ds by ing of ellow- t Cancelled U.S. Federal Methods. 2.2 U.S. Federal Test Method Standard J41:12 1022 Sampling (General) 2131 Application of Sprayed Films 2141 Application of Brushed Films 3011 Condition in Container 3021 Skinning (Partially Filled Container) 4042 Volatile and Nonvolatile Content (Vacuum Oven) 4321 Brushing Properties. 4331 Spraying Properties 4335 Roller Coating Properties 4421 Absorption Test 4541 Working Properties and Appearance of Dried Film 3. Definitions 3.1 For definitions of terms in these practices, refer to Definitions D 16 and D 1554. L Conditions Affecting Solvent-Thinned Flat Wall Paint Topcoats 4.1 Practical requirements and performance of solvent- thinned flat wall paints may vary with: 4.1.1 Substrate Type, such as type and quality of wood or i 12 Available from Standardization Documents Order Desk, Bldg. 4 Section D, I ''""I Robbins Ave., Philadelphia, PA 19111-5094. t hardboard, wallboard and joint cement systems, alkalinity, type and quality of plaster, and type and quality of old paint. 4.1.2 Substrate Conditions--Smoothness of substrate and quality of topcoat will affect spreading rate, final appearance, and texture. 4.1.3 Type and quality of primer and the time before topcoating. 4.1.4 Environmental conditions, such as temperature and humidity, at the time of paint application and during drying. 5. Sampling 5.1 Prior to sampling, the condition of the container should be established since damage to it may cause evapora tion, skinning, or other undesirable effects in the coating. Determine the condition of the paint in accordance with 6.1 and 6.2. 5.2 Sample in accordance with Section 4.2.1 of Method 1021 of Federal Test Method No. 141. Determine the weight per gallon in accordance with Test Method D 1475. Repeat this procedure until successive values agree within 0.1 lb (45 g) or as agreed upon between the purchaser and the seller. Then take samples for testing. 5.3 Specify die amount of sample, the package sizes, and identification codes to assure a representative sample. A 465 w !} * r r L DU P0502 97646 # D 3323 TABLE 2 Alphabetical List of Test Methods Test Method Section ASTM Test Method Absorption test Adhesion Application of brushed films Application of sprayed films Coarse particles and foreign matter Color acceptance Color difference by visual comparison Color difference by instrument evaluation Condition in container Consistency Drying time Elongation Fineness of dispersion Flash point Fume resistance Hiding power (dry opacity) Identification of vehicle solids Leveling properties Pigment content Producing films of uniform thickness Rheological properties of non-Newtonian materials Roller coating properties Sampling Scrub resistance Separation of vehicle Skinning Specular (gloss sheen) Volatile content Washability Water content Weight per gallon Working properties Yellowness index 6.10 9.1 7.1 7.2 6.3 6.8 8.1 8.2 62 6.6 7.3 93 6.4 6.7 9.4 8.4 10.6 7.4 10.4 7.5 6.9 7.6 S 92.1 10.5 6.1 8.3 10.2 9.2.2 10.3 6.5 7.7 9.5 D 2197 D185 D 1729 D 2244 562 D 1640 D 1737, D 522 D1210 D1310, D 93, D 3278 2805,D 344 D 2621 D 2801 D 2371 D 823 D 2196 E105 2486 2372 154 523 2369 1208 D 1475 E 313 Federal Test Method's^ No. 141 4421 6303 2141,4321 2131,4331 4091 jj |' 4249 6123 3011 4281 4061 6221 4411 ! ii if t i 1s 1 ? JJ' 4021,4022 2162 4335 1022 4032 3021 6103 4041.4042 6141 4081 4184 4541 6131 1 i1 'i F *; ; Ji ' 41 ( "1* [ 1-gal (4-L) sample is usually sufficient for the recommended tests, but for guidance in selecting a sampling plan, consult Recommended Practice E 105. 6. Liquid Paint Properties 6.1 Skinning--Paints containing a binder which dries by oxidation are subject to skin formation in a partially filled can. Since skins are insoluble in the paint, they must be removed before use. This test in a partially filled container indicates the tendency of a paint to skin. Examine the original sample for skins, both on the surface and in its mass. On a well-mixed, skin-free portion of the sample, perform a skinning test in accordance with Guide D 154. 6.2 Condition in Container--Thickening, settling, and separation are undesirable and objectionable if the paint cannot be reconditioned with a reasonable amount of stirring. The referenced method covers procedures for deter mining changes in properties of paints after storage. Deter mine the condition in the container in accordance with Method 3011 of U.S. Federal Test Method Standard No. 141. 6.3 Coarse Particles and Foreign Matter--Paints must be free of coarse particles and foreign matter to form a uniform film of good appearance, a typical maximum being 1 weight % of the total paint. Determine the percent of coarse particles and foreign matter in accordance with Test Method D 185. 6.4 Fineness ofDispersion--The more finely a pigment is dispersed the more efficiently it is being utilized. One method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the product down a tapered groove varying in depth from 4 to 0 milf) (100 to 0 pm). The point at which continuous groupings of;: particles or agglomerates, or both, protrude through tlf, l surface of the wet film is taken as the dispersion res Higher readings in Hegman units or lower readings in mils or micrometres indicate better dispersion. Determine the fine-, ness of dispersion in accordance with Test Method D 1210." 6.5 Weight per Gallon--The density of a paint as mea: sured by weight per gallon or kilograms per litre is used to assure product uniformity, batch to batch, and provides check against the theoretical weight calculated from the! formula. The density is expressed as the weight in pound! avoirdupois of 1 U.S. gal of the paint at a specified temperature. Determine weight per gallon or kilograms pet; litre in accordance with Test Method D 1475, using i calibrated weight per gallon cup. 6.6 Consistency--Paints of a given type should fall within' a stated consistency range for satisfactory reproduction oflj specific formula. In the referenced test method, consistency is defined as the load in grams required to produce th< specified rate of shear. Determine consistency in accori with Test Method D 562. 6.7 Flash Point--When the flash point of a material is required for shipping information, use Test Method^ D 1310, D 3278, orD93. ; 6.8 ColorAcceptance--This method gives an indication c the ability of the paint to be tinted with tinting systems a common use. Determine color compatibility as agreed upff1lf ! between the purchaser and seller. ti 6.9 Rheological Properties ofNon-Newtonian Materials--^ Rheological properties are related to application and flo*l \ 466 DUP0502 97647 Mod Sttj, 21 .31 '22 )42 to 0 mils upings of ough the reading, in mils or the fineD 1210. as meai used to ivides a om the pounds pecified ims per using a all within ;tion of a insistency iduce the xordance laterial is Methods .ication of ystems in -eed upon aterials-- and flow # D 3323 ^operties of the liquid paint. The referenced test method jpvers the determination of the rheological properties and is .jjticularlv suited for use with paints that display thixotropic Jjjaracteristics. Determine the rheological properties in accprdance with Test Method D 2196. 6.10 Absorption--This method provides a rapid determi nation of the relative penetration of the binder into the juiface. It provides a rough measure of the wetting and penetrating properties of liquid materials. Loss of binder and resultant change in pigment volume, as the film dries, are indicated by this test. Determine the absorption in accord ance with Method 4421 of U.S. Federal Test Method Standard No. 141. 7, Paint Application and Filin Formation 7.1 Application ofBrushed Films--Refer to Method 2131 or 4321 of U.S. Federal Test Method Standard No. 141 to determine the brushing properties of a coating. Method 4321-1 is quite subjective although someone experienced in tiie art can obtain consistent results, particularly in the determination of the "drag" properties. 7.2 Applications of Sprayed Films--Refer to Method 2131 or 4331 of U.S. Federal Test Method Standard No. 141 to determine the spraying properties of a coating. Method 4331 is very subjective and should be performed by an individual skilled in the art of using spray equipment. 7.3 Drying Time--The drying time of an interior finish is important in determining when a freshly painted room can be put back to use. The test can also be used to determine whether or not the drying properties of a paint have changed during storage. Any one or several of the test methods that cover the determination of the various stages and rates of film formation in the drying or curing of organic coatings may be used. For example, if two coats are specified, the determination of "dry-to-recoat" times will be important. Determine the appropriate drying time in accordance with Test Method D 1640. 7.4 Leveling Properties--Leveling is an important factor when smooth surfaces are to be produced. The referenced test method covers the laboratory determination of the relative leveling characteristics of liquid coatings. Determine leveling characteristics in accordance with Test Method D2801. 7.5 Producing Films of Uniform Thickness--Method D823 covers the preparation of coating films of uniform thickness essential in conducting tests. 7.6 Roller Coating Properties--The referenced method outlines a procedure for making an evaluation of a material's characteristics when applied by a roller. Determine roller coating properties in accordance with Method 4335 of U.S. Federal Test Method Standard No. 141. 7.7 Working Properties--Working properties of a paint are generally compared to a standard or described by re quirements in the product specification. Determine work ing properties in accordance with Method 4541 of U.S. Federal Test Method Standard No. 141. 8. Appearance of Dry Paint Film 8.1 Color Difference ofOpaque Materials by Visual Com parison--Visual comparison of color is fast and often acceptable. The referenced practice covers the spectral. photometric, and geometric characteristics of light source, illuminating and viewing conditions, sizes of specimens, and general procedures to be used in the visual evaluation of color differences of opaque materials. Determine color difference in accordance with Practice D 1729. 8.2 Color Differences of Opaque Materials by Instrument Evaluation--Color difference between a product and the standard can be measured by instrument. The referenced method covers the instrumental determination of small color differences, observable in daylight illumination, between nonfluorescent, nonmetameric, opaque surfaces such as paint specimens. If metamerism is suspected, visual evalua tion (8.1) should be used to verify instrumental results. Determine the color difference in accordance with Method D 2244. 8.3 Specular Gloss (Sheen)--The test method given, using the 85 geometry, is useful in characterizing the low angle appearance of flat paints. Determine 85 gloss in accordance with Test Method D 523. 8.4 Hiding Power--Hiding power is a measure of the ability of a coating to hide the substrate. It is, however, dependent on uniform film thickness which is influenced by the flow, leveling, and application properties of the enamel. Test Method D 344 uses brush application and compares the enamel to a standard. Test Method D 2805 uses an appli cator, bar and is more reproducible and measures smaller differences than D 344. Determine hiding power in accord ance with Test Methods D 344 or D 2805. 9. Properties of Dry Paint Film 9.1 Adhesion--Measure the adhesion of the paint by testing in accordance with Test Method D 2197. 9.2 Cleanability--The ability to remove marks satisfacto rily without damaging the film is important with interior finishes. 9.2.1 Scrub Resistance--The test for scrub resistance of interior latex flat wall paint can be applied to the solventthinned type. Use Test Method D 2486. 9.2.2 Washability--The referenced method determines the washability of a paint by subjecting a soiled film of the dried paint to the cleaning action of a wet sponge and cake grit soap. Determine the washability in accordance with Method 6141 of U.S. Federal Test Method Standard No. 141. 9.3 Elongation--Elongation is a measure of flexibility of a paint film. Determine elongation in accordance with Test Methods D 1737 or D 522. 9.4 Fume Resistance--Some paints exhibit a change in appearance (usually color) when subjected to foul atmos pheres, for example, air containing certain sulfur com pounds. There is no standard test method for determining the ability of a paint to resist this change. 9.5 Yellowness Index--The referenced test method is used for white or near white specimens to determine color departure from white toward yellow or color change towards yellow on exposure or treatment. Determine the yellowness index in accordance with Test Method E 313. 10. Analysis of Paint 10.1 If a specification requires certain raw materials or certain components in a given amount, then chemical 467 DUPO 502 97648 D3323 D analysis is required. Chemical analysis determines whether the specified components are present and if they are, in what amounts. It does not necessarily establish paint quality which can be greatly affected by manufacturing techniques. No single schematic analysis is comprehensive enough to cover the wide variety of materials used in paint compositions. 10.2 Volatile Content--The percent of volatile matter indicates the thinner loss from the film as it dries. The referenced test method covers the determination of the volatile content of solvent-type paints. The quantity deter mined subtracted from 100 % gives the nonvolatile content of the coating. Determine the volatile content in accordance with Test Method D 2369. 10.3 Water Content--The referenced test method covers the determination of water in paint and related materials by distilling the sample with a volatile solvent. Determine water content in accordance with Test Method D 1208. 10.4 Pigment Content--'Pigment provides the hiding and color and influences many other properties of a coating. The referenced test method describes the procedure for the quantitative separation of the vehicle from the pigment in solvent-type coatings. It is used to determine the weight percent pigment in the paint. Determine the pigment content in accordance with Test Method D 2371. 10.5 Separation of Vehicle--The recommended proce dure describes the separation of vehicle from certain solventtype paints. The separated vehicle is subjected to further analysis. Separate the vehicle in accordance with Method D 2372. 10.6 Identification of Vehicle Solids--The suggested method covers the qualitative characterization or identifica tion of separated paint vehicle solids by infrared spectros copy. It is useful in detecting uniformity, batch to batch, and the presence of adulterants. Characterize vehicle solids in accordance with Method D 2621. The American Society for Testing amt Materials takas no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments ere Invitedeitherfor revision ofthis standard or for additionst standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have net received a fair hearing you should make your views known to the ASTM Committee on Standards, 191B Race St., Philadelphia, PA 19103. Scope l.l T1 contents 50 and and 200< liquid c reason t not be appropr reagent 1.2 C test me and lac that ap 1.3 ' tion of recove 1.4 form c than ( slight) 1.5 safeti respo priau bility state' 2. R 2. D D and mint C Orig 2 Con Ma> 468 . ..rflk,- DU P05 02 97649 S anjj s-The r the -nt 'eight coo. %I s3 !; Designation: D 3335 - 85a (Reapproved 1991)t Standard Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy1 >roce. vent. irther -thod ssted ifica- *ros. >and ds in This standard is issued under the fixed designation D 3335; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the Department of Defense. Consult the DoD index of Specifications and Standards for the specific year ofissue which has been adopted by the Department ofDefense. Note--Keywords were added editorially in June 1991. 1. Scope 1.1 This test method covers the determination of lead2 intents between 0.01 and 5 %, cadmium contents between 50 and 150 ppm (mg/kg), and cobalt contents between 50 and 2000 ppm (mg/kg) present in the nonvolatile portion of liquid coatings or contained in dried films. There is no [gason to believe that higher levels of all three elements could DOt be determined by this test method, provided that appropriate dilutions and adjustments in specimen size and jeagent quantities are made. 1.2 Only pigmented coatings were used for evaluating this test method, but there is no reason to believe that varnishes and lacquers could not be analyzed successfully, provided that appropriate precautions are taken. 1.3 This test method is not applicable to the determina tion of lead in samples containing antimony pigments (low recoveries are obtained). 1.4 If lead is present in the sample to be analyzed in the form of an organic lead compound at a concentration greater than 0.1 %, small losses of lead may occur, resulting in slightly poorer precision than shown in Section 12. 1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. Specific hazard statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water3 D 2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings4 3. Summary of Test Method 3.1 The specimen of liquid coating or dried film is prepared for 'analysis by dry ashing. The content of lead, cadmium, or cobalt of an acid extract of the ash is deter mined by atomic absorption spectroscopy. 4. Significance and Use 4.1 The permissible level of heavy metals in certain coatings is specified by governmental regulatory agencies. This test method provides a fully documented procedure for determining low concentrations of lead, cadmium, and cobalt present in both water and solvent-reducible coatings to determine compliance. 5. Apparatus 5.1 Atomic Absorption Spectrophotometer, consisting of an atomizer and either a single- or three-slot burner; gas pressure regulating and metering devices for air and acety lene; lead, cadmium, and cobalt source lamps5 with a regulated constant-current supply; a monochromator and associated optics; a photosensitive detector connected to an electronic amplifier; and a readout device. 5.2 Muffle Furnace, capable of maintaining 500 10C. 5.3 Crucibles, wide-form, porcelain, glazed inside and outside except for the outside bottom surface, approximately 30-mL capacity, 50-mm rim diameter and 31-mm height.6 5.4 Hot Plate, with variable surface temperature control over the range from 70 to 200C. 5.5 High-Silica Glass Beakers,7 100 and 250-mL. 5.6 Volumetric Flasks, 50, 100, and 1000-mL. 5.7 Dropping Bottles, }A or 'A-oz (7 or 15-mL) capacity. 5.8 Glass or Disposable Syringes, 5 or 10-mL capacity. 5.9 Pipets, 1, 2, 5, and 10-mL capacity. 5.10 Paint Shaker. 5.11 Paint Draw-Down Bar. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. ] Current edition approved July 16 and Nov. 29, 1985. Published January 1986. j Originally published as I> 3335 - 74. Last previous edition D 3335 - 84. 2 Vandeberg, J. T., Swafford, H. D,, and Scott, R. W., "Determination of Low j Concentrations of Lead in Paint," Journal ofPaint Technology, Vol 47, No. 604, j % 1975, 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Annual Book ofASTM Standards, Voi 06.01. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be 5 Both hollow cathode lamps and electrodeless discharge lamps have been found satisfactory for this purpose. 6 Coors No. 25007 crucibles, or equivalent, have been found satisfactory for this purpose. 7 Vycor beakers manufactured by the Coming Glass Co. have been found satisfactory for this purpose. ft 469 DUP050297650 i>s9Z62osodna QLP moij jsapsq > 6 sjqpnjs sqj 7 89< 7> `(q Z l I pssaxs i ||u op) sjsjduios sq oj sresddB SuiqsB sqj usq/^ 9*5 uoaBztjijE]OA Aq pBS[ suios jo sso] :^ ui l[nssj A' < D.OOS Js s s s x s in samjBJSduisi > ' Suiqsy--p 310N 'DoOOS I SLP18 qsn puB ;<' ==< > sujnui psjBsqsid Jfcn >?> < ' > ?@o sqj ooBjd `sjsjduioo si SuuiBqo isyy S'6 'sjBqo ppsjEai sqj [rjun sjBjd joq iqj jo sinjnjsdaisj sqj AA' A> BC< AjpenpcjS `uqg psup ' qjiM |ipiBis asqM > D Ajp sq oj siBSdds usuipsds sqj usq^ P'6 'Suusjjeds oj 3np S3SS0] Sauinou; jnoqjiM E> FE > o s SAOUISJ OJ AJBSS333U 3q ABUI 3o$0l l SuiAjp-USAO IBIJiai m G`sS < > ' Hojo ssdAj suios qji^ -psup si [' IJ> ' I< sq: quin |miBJ3dUI3J Sqj SSBSJSUI AlMOp pUB SJBjd JOq B UO SUIJBOD j |mbii sqj SK<K< ' > KLL(isjjBsq > M) sjqptus sqj 33B[<j '6 I 1 '3pB|q NO> ' : sSps-sfSuis ' qjiM A[qEisjaid `siE[d s s' ( sqi jyo \ |s[y paup sqi sdBs '4 l J uinuiiuiui ' P> > 3,501 I U3A0 UB u! 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Heat carefully on a hot plate until 2 to 3 mL of solution remain. Add an additional 10 mL of HNOs (1 + 1) and continue heating on the hot plate until less than 5 mL of the solution remains. 9.8 Filter the solution through medium-porosity filter paper into a 50-mL volumetric flask. If the filtrate is not clear, refilter through fine-porosity filter paper. Wash the container three times with 2.5 mL of hot ammonium acetate solution (6.3), each time transferring the washings to the glter paper. Wash the filter paper several times with water, adjust the volume to 50 mL with water and mix. 9.9 Aspirate the test solution and determine the absorbance in the same manner in which the instrument was calibrated. Determine the concentration of lead, cadmium, or cobalt in micrograms per millilitre from the calibration curve. If the absorbance is above the range covered by the calibration curve, dilute an aliquot of the sample solution to a suitable volume with ammonium acetate diluting solution. No t ' 5--For maximum accuracy, calibration and standardization (Section 8) should be completed just prior to aspirating the sample solution. N' 6--The method of standard additions may be used to improve the accuracy of the analysis. This method is particularly recommended for use with unknown samples where matrix effects may be potentially significant. For a detailed description of the procedure and calculations used in the method of standard additions, consult a standard text on atomic absorption spectroscopy or the instruction manual provided by the instrument manufacturer. 10. Calculation 10.1 Calculate the mean concentration of lead, cadmium, or cobalt in the nonvolatile portion of the sample as follows: lead, cadmium or cobalt, ppm (mg/kg) in nonvolatile = (CxFx 5000)/(NVx S) where: C = concentration of lead, cadmium, or cobalt in the aspirated specimen solution, (pg/mL), F -- dilution factor from 9.9 (volume diluted to/volume of aliquot), 5000 = factor derived from multiplying the 50-mL volume obtained in procedure in 9.8 by 100 (to convert NV used to a whole number) and 10 (to obtain ppm), then dividing by 106 (to convert grams of sample to H8). NV = percent nonvolatile of paint sample (use 100 if sample was a dried film), and S = sample, g. 11. Report 11.1 Report the lead, cadmium, or cobalt content of the nonvolatile content of'the sample and whether the analysis was conducted on a liquid coating or a dried film. 12. Precision and Bias9 12.1 The precision estimates are based on an inter laboratory study in which seven different laboratories ana lyzed in duplicate, on two different days, four samples of water-reducible paints and four samples of solvent-reducible paints containing from 0.01 to 5 % lead, 50 to 150 ppm (mg/kg) cadmium, and 50 to 2000 ppm cobalt. The withinIaboratory coefficient of variation was found to be 3.4 % relative at 24 degrees offreedom for lead, 3.7 % relative at 15 degrees of freedom for cadmium, and 3.3 % relative at 21 degrees of.freedom for cobalt. The between-laboratory coef ficient of variation was 9.3 % relative at 20 df for lead, 8.9 % relative at 11 df for cadmium, and 5.5 % relative at 17 df for cobalt. Based on these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 12.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 11 % relative for ail three metals. 12.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 28 % relative for lead or cadmium or by more than 17 % relative for cobalt. 12.2 Bias: 12.2.1 The true value for the amount of lead present in the solids of a coating should be between 97 and 111 % of the experimental value. , 12.2.2 The true value for the amount of cadmium present in the solids of a coating should be between 77 and 143 % of the experimental value. 12.2.3 The true value for the amount of cobalt present in the solids of ia coating should be between 96 and 120 % of the experimental value. 13. Keywords 13.1 AAS trace metals in paints; trace cobalt paints; trace lead cadmium paints; trace lead in paints 'Supporting data are available from ASTM Headquarters. Request, RR: D01-1005. :n starting ure of the finer in a j \ result in dw : ; (do not from the The American Society lor Testing and Materials takas no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthisstandard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ofWe responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. -................. --................... 471 DUP050297652 Designation: D 3358 - 88 Standard Guide for Testing Water-Borne Floor Paints1 This standard is issued under the fixed designation D 3358; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the Department of Defense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been approvedfor use by the Department ofDefense. E7C G EK 2.2 102 212 214 301 432 433 1, Scope 3- Co D659 Test Methods for Evaluating Degree of Chalking o( Pa 1.1 This guide covers the selection and use of procedures for testing water-borne floor paints. The test methods in cluded are listed in Tables 1 and 2. N' --Where no ASTM test method exists ot there is a comparable (but not necessarily identical) method in Federal Test Method Standard, No. 141, the Federal Method number is listed. However, the Federal Method shall not be considered approved by ASTM. 1.2 The guide covers the testing of ready-mixed finish coats applied by brush or roller on surfaces subjected to traffic, such as floors, decks, platforms, stairs, and adjacent surfaces such as stair risers and railings. 1.3 Floor paints may be intended for interior use only or may also be suitable for use on exterior surfaces exposed to the weather, such as decks, porches, porch steps, and carport floors. Paints intended for both exterior and interior use require certain test procedures not applicable to paints in tended for interior use only. Selection of test methods must be governed by the requirements in each individual case, together with agreement between the purchaser and the seller. 2. Referenced Documents 2.1 ASTM Standards: D16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 Exterior Paints4 D 660 Test Methods for Evaluating Degree of Checking of Exterior Paints4 D 661 Test Method for Evaluating Degree of Cracking of Exterior Paints4 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints4 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints4 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels4 D 968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive4 D1006 Practice for Conducting Exterior Exposure Tests of Paints on Wood4 D1210 Test Method for Fineness of Dispersion of Pigment Vehicle Systems4 D 1308 Test Method for Effect of Household Chemical on Clear and Pigmented Organic Finishes4 D 1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products4 D 1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature4 D1729 Practice for Visual Evaluation ofColor Differences 3.1 water 3.1 conci borni surfa 3.1 smoe Clea; can i 3. hum thest have temi fom 3. that or i blisi 4. 1 4 Dei D 185 Test Methods for Coarse Particles in Pigments, of Opaque Material5 i* Pastes, and Paints3 D1737 Test Method for Elongation of Attached Organic 5. . D215 Methods ofChemical. Analysis of White Linseed Oil Coatings with Cylindrical Mandrel Apparatus6 Paints4 D1848 Classification for Reporting Paint Film Failures sh> : -M D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts4 D358 Specification for Wood to Be Used as Panels in Characteristic of Exterior Latex Paints4 D1849 Test Method for Package Stability of Paint4 D 219? Test Method for Adhesion of Organic Coatings by tic De an Weathering Tests of Coatings4 Scrape Adhesion4 D 522 Test Methods for Mandrel Bend Test of Attached D 2243 Test Method for Freeze-Thaw Resistance of Latex 10. Organic Coatings4 D 523 Test Method for Specular Gloss4 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer4 D658 Test Method for Abrasion Resistance of Organic and Emulsion4 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates4 D 2369 Test Method for Volatile Content of Coatings4 D 2574 Test Method for Resistance of Emulsion Paints in pei Mt agi ch Coatings by Air Blast Abrasive4 the Container to Attack by Microorganisms4 D2805 Test Method for Hiding Power of Paints by id< 1- Reflectometry4 bi 1 This guide is under the jurisdiction of ASTM Committee D-l on Paint and D 4062 Test Method for Leveling of Paints by Draw-Down Pi Related Coatings and Materials and is the direct responsibility of Subcommittee D 01.42 on Architectural Finishes. Method4 Current edition approved March 25, 1988. Published May 1988. Originally published asD3358-74. Last previous edition D 3358 - 79.- - 2 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 1 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 5 Annua! Book ofASTM Standards, Vol 14.02. 6 Discontinued; see 1988 Book ofASTM Standards, Vol 06.01. Replaced by 70 * Annual Book ofASTM Standards, Vol 06.01. Test Method D 522. 472 DU PO50297653 igof IgOf Ig Of m of iking form ts on ganic StS of ~ Pigjalon , Lacormarences ganic lures gsby Latex rences 4 gs4 nts in its by Down laced by D 3358 70 Test Method for pH of Aqueous Solutions with the Glass Electrode7 E 105 Practice for Probability Sampling of Materials5 2.2 US. Federal Test Method Standard 141* 1021 Sampling (General) 2121 Application of Dipped Films 2141 Application of Brushed Films 3011 Condition in Container 4321 Brushing Properties 4335 Roller Coating Properties 3. Conditions Affecting Performance of Water-Borne Floor Paints 3.1 Practical requirements affecting and performance of water-thinned floor paints may vary with; 3.1.1 Substrate type, such as type and quality of wood, concrete, metal, or composition flooring. The use of water borne floor paints is generally restricted to previously painted surfaces or unpainted concrete. 3.1.2 Substrate conditions such as porosity, hardness, smoothness, or in the case of unpainted concrete, alkalinity. Cleanliness is very important as traces of oily contaminants can cause water-borne floor paints to peel. 3.1.3 Environmental conditions such as temperature and humidity at the time of application and during drying. As these paints contain water as a. thinner, the floor does not have to be completely dry before application. However, low temperature during the drying period may cause poor film formation. 3.1.4 Substrate Aspects--If construction defects are such that excessive moisture makes its way through the substrate, or if the substrate is in direct contact with damp ground, blistering, flaking, or peeling may result. 4. Definitions 4.1 For definitions of terms used in this guide, refer to Definitions D 16. 5. Sampling 5.1 Prior to sampling, the condition of the container should be established since damage to it may cause evapora tion, skinning, or other undesirable effects in the coating. Determine the condition of the paint in accordance with 6.1 and 6.2. 5.2 Sample in accordance with Section 4.2.1 of Method 1021 of Federal Test Method No. 141. Determine the weight per gallon (or kilograms per litre) in accordance with Test Method D 1475. Repeat this procedure until successive values agree within 0.1 lb (45 g) or as agreed upon between the pur chaser and the seller. Samples for testing may then be taken. 5.3 Specify the amount of sample, the package sizes, and identification codes to assure a representative sample. A 1-gal sample is usually sufficient for the recommended tests, but for guidance in selecting a sampling plan, consult Practice E 105.* 6 ' Annual Book ofASTM Standards, Vol 15.05. 6 Available from Standardization Documents Order Desk, Bldg. 4 Section t), ?00 Robbins Ave., 19111-5094. TABLE 1 Ust of Test Methods by Properties Test Method Liquid Paint Properties: Condition In container Course particles and foreign matter Density or weight per gallon Fineness of dispersion Consistency pH measurement Freeze-thaw resistance Package stability Resistance to microorganisms Paint Application and Film Formation: Application of brushed film Brushing properties Roller coating properties Orying properties Leveling properties Producing films of uniform thickness. Appearance of the Dry Film: Color difference of opaque materials, visual evaluation of Color difference of opaque materials, instrumental evaluation of Gloss Hiding power Properties of the Dry Rim: Abrasion resistance Elongation (flexibility} Adhesion Resistance to chemicals Exterior exposure Conducting exterior exposures and Reporting film features characteristic ot exterior latex paints Wood panel description Chalk resistance Checking resistance Cracking resistance Erosion resistance Flanking resistance Analysis of Paint: Chemical analysis Volatile content Pigment analysis Section ASTM Method Federal Test Method Standard No. 141 6.1 3011 65 0185 6.3 D1475 6.4 D1210 6.5 D 562 6.6 E70 67 D2243 6.8 D1849 6.9 D2574 7.1 2141 7.2 4321 7.3 4335 7.4 D 1640 7.5 D 4062 7.6 D 823 8.1 D1729 8.2 D 2244 8.3 8.4 9.1 9.2 9.3 9.4 9.5 9.5.1 9.5.1 D 523 D 2805, D 344 D 658, D968 0 522, D1737 D2197 D 1308 6221 D 1006 D 1848 9.5.2 9.5.3 9.5.4 9.5.5 9.5.6 9.57 10.1 10.2 10.3 D358 D659 D 660' D 661 D 662 D 772 D 2369 D 215 6. Liquid Paint Properties 6.1 Condition in Container--Thickening, settling, and separation are undesirable and objectionable if a paint cannot be reconditioned and made suitable for application with a reasonable amount of stirring. The referenced methods covers procedures for determining changes in properties of paints after storage. Determine the condition in the container in accordance with Method 3011 of Federal Test Method Standard No.' 141. 6.2 Coarse Particles and Foreign Matter--Paints must be free of coarse particles to form uniform films of good appearance, a typical maximum being 1 weight % of total paint. The specified test with a No. 325 (45-pm) sieve gives the percent of these particles in a paint. Determine coarse particles and foreign matter in accordance with Test Methods D 185. r r r r r r r ( k. 473 DUP0502 97654 T # 0 3358 TABLE 2 Alphabetical List of Test Methods Test Method Abrasion resistance Adhesion Application of brushed films Brushing properties Chalk resistance Checking resistance Chemical analysis Coarse particles and foreign matter Color differences of opaque materials. instrumental evaluation of Color differences of opaque materials. visual evaluation of Condition in container Conducting exterior exposures Consistency Cracking resistance Density or weight per gallon Drying properties Elongation Erosion resistance Exterior exposure Fineness of dispersion Flaking resistance Freeze-thaw resistance Gloss Hiding power Leveling properties Package stability pH measurement Pigment analysis Producing films of uniform thickness Reporting pant film features, characteristic of exterior latex paints Resistance to microorganisms Resistance to chemicals Roller coating properties Volatile content Wood panel description Section 9.1 9.3 7.1 7.2 9.5.3 9.5.4 10.1 6.2 8.2 ASTM Method D 658, D 968 D 2197 D 659 D 660 Federal Test Method Standard No. 141 2141 4321 6421 O 185 0 2244 8.1 D 1729 4249 6.1 9.5.1 6.5 9.5.5 6.3 7.4 9.2 9.5.6 9.5 6.4 9.5.7 6.7 8.3 8.4 7.5 6.8 6.6 10.3 7.6 9.5.1 D1006 D 562 D661 D 1475 D 1640 0 522, D1737 D662 D 1210 D 772 0 2243 D 523 0 2805, D 344 D4062 D 1849 B 70 D 215 D823 O 1848 3011 6471 6221 6.9 9.4 7.3 10.2 9.5.2 D 2574 D1308 0 2369 D 358 4335 6.3 Density or Weight per Gallon--The density as mea sured by weight in pounds per gallon (kilograms per litre) is used to assure product uniformity from batch to batch. In the referenced method, density is expressed as the weight in pounds of 1 U.S. gal (or kilograms per litre) of the paint at a specified temperature. Determine density in accordance with Test Method D 1475 using a.calibrated cup. 6.4 Fineness ofDispersion--The more finely a pigment is dispersed, the more efficiently it is being used. One method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the material down a calibrated, tapered groove in a hardened, steel block with the groove varying in depth from 4 to 0 mils (100 to 0 pm) and calibrated Hegman 0-8. The point at which continuous groupings of particles or agglomerates, or both, are visible through the surface of the liquid is taken as the fineness reading. Lower readings in mils or pm or higher readings in Hegman units indicate better fineness of dispersion. Deter mine fineness of dispersion in accordance with Test Method D 1210. 6.5 Consistency--Consistency is important, relating to application and flow, and should fall within a range agreed upon. In the referenced method consistency is defined as the load in grams required to produce a specified rate of shear and also expressed in Krebs units. Other methods may used as agreed upon between the purchaser and the seller Determine consistency in accordance with Test Method D 562. 6.6 pH--The pH of a water-thinned paint depends on the type of latex used and the general formulation. It may vary from about 5 to 10. pH does not determine the quality of% paint and should not be used to assure product uniformity. 4 change in pH during storage may indicate poor stability ora change in properties of a water-thinned paint. Determine pft in accordance with Test Method E 70. 6.7 Freeze-Thaw Resistance--Water-thinned paints may be subjected to freezing conditions during shipping and storage. Suitably stabilized paints resist several cycles of freezing and thawing without showing deleterious changes. The referenced method covers the determination of the extent to which water-thinned floor paints, utilizing synthetic latices or synthetic resin emulsions as vehicles, retain their original properties when subjected to freezing and subse. quent thawing. Determine freeze-thaw resistance in accordance with Test Method D 2243. 6.8 Package Stability--Since paints cannot normally be used immediately after manufacture, they must remain stable in the can for some time. At normal temperatures, most water-thinned floor paints can be stored for over a year with little change in properties. The referenced method covers the change in consistency and in certain related properties that may take place in packaged latex paint when stored at temperatures above freezing. Determine package stability in accordance with Test Method D 1849. 6.9 Resistance to Microorganisms--Bacteria in a water borne floor paint can cause gassing, putrefactive or fermen tative odors, and loss of viscosity. Determine if the paint contains living bacteria and if it is resistant to attack by bacteria in accordance with Test Method D 2574. 7. Paint Application and Film Formation 7.1 Application of Brushed Films--Brushed films should be smooth and free of seeds, color streaking, and brush marks. Test brush application in accordance with Method 2141 of Federal Test Method Standard No. 141. 7.2 Brushing Properties--The specified method covers a means for determining the brushing properties of coatings. The test is quite subjective; however, someone experienced in the art can produce quite consistent results, particularly in the determination of "drag" qualities. Floor paints are generally applied to horizontal surfaces but evaluation on vertical surfaces may be necessary to determine performance on stair risers, railings, posts, baseboards, etc. Determine the brushing properties in accordance with Method 4321 of Federal Test Method Standard No. 141. 7.3 Roller Coating Properties--Floor paints are frequently applied by roller. The referenced method outlines a proce dure for evaluating a material's characteristics when applied by a roller. Determine roller coating properties in accordance with Method 4335 of Federal Test Method Standard No. 141. 7.4 Drying important in stair may be s result in dust exterior surf; appearance, to-touch in 1 film. Detern Methods D 1 7.5 Levelif when unifom and appearar tory determir liquid coating ance with Te: 7.6 Prodm Methods D S uniform thicl 8- Appearam 8.1 Color uation--Visi able althoug referenced n geometric ch; viewing cone dures to be u of opaque m ance with Pr; 8.2 Color mental Evah the standard tolerance is seller. The instrumental servable in < nonmetamer metamerism used to ve: difference r Method D 2 8.3 Gloss semi-gloss fi proves wash, typical. Dete Methods D; 8.4 Hidin. measure of; however, do influenced b practical tes; thickness is visually as c affected by paint. Test precise andt standard. Pa the effects o measured, a 474 DUP050297655 the shear *y be eller. :thod nthe vary the ty. A ora epH may and iS Of ages. the hetic their lbse:ord- y be nain ures, year thod lated vhen kage aternen>aint c by uld ish tod ;rs a ngs. iced ly in are i on ince : the 1 of ntly oce llied mce No. D3358 7.4 Drying Properties--The drying time of a floor paint is important in determining when a freshly painted floor of stair may be subjected to traffic. Slow drying of the film may result in dust pickup, poor appearance and, if used on an exterior surface, rain or dew may cause a nonuniform appearance. Generally, water-thinned paints are dryto-touch in 1 or 2 h when the water has evaporated from the film. Determine drying time in accordance with Test Methods D 1640. 7.5 Leveling Properties--Leveling is an important factor when uniform surfaces are to be produced, as it affects hiding and appearance. The referenced method covers the labora tory determination of the relative leveling characteristics of liquid coatings. Determine leveling characteristics in accord ance with Test Method D 4062. 7.6 Producing Films of Uniform Thickness--Test Methods D 823 covers the preparation of various films of uniform thickness essential in conducting tests. 8. Appearance of the Dry Film 8.1 Color Difference ofOpaque Materials by Visual Eval uation--Visual comparison of color is fast and often accept able although numerical values are not obtained. The referenced method covers the spectral, photometric, and geometric characteristics ofthe light source, illuminating and viewing conditions, size of specimens, and general proce dures to be used in the visual evaluation of color differences of opaque materials. Determine color difference in accord ance with Practice D 1729. 8.2 Color Differences of Opaque Materials by Instru mental Evaluation--Color difference between a product and the standard can be measured by instrument Generally the tolerance is agreed upon between the purchaser and the seller. The referenced method covers the calculation of instrumental determinations of small color differences, ob servable in daylight illumination, between nonfiuorescent, nonmetameric, opaque surfaces such as coated specimens. If metamerism is suspected, visual evaluation (8.1) should be used to verify instrumental results. Calculate the color difference measured instrumentally in accordance with Method D 2244. 8.3 Gloss--Water-thinned floor paints generally have a semi-gloss finish which resists penetration of dirt and im proves washability. A range from 20 to 40 may be considered typical. Determine the specular gloss in accordance with Test Methods D 523. 8.4 Hiding Power (Dry Opacity)--Hiding power is the measure of the ability of a paint to hide the substrate. It is, however, dependent upon uniform film thickness which is influenced by flow and leveling. Test Method D 344 is a practical test in which paint is applied with a brush, film thickness is approximately measured, opacity is evaluated visually as compared to a standard paint, and results are affected by flow and leveling application properties of the paint. Test Method D2805 is considered to be a more I precise and accurate test that does not need a material paint standard. Paint is applied with an applicator bar to minimize the effects of flow and leveling, film thickness is rigorously measured, and opacity is instrumentally evaluated. Deter mine hiding power in accordance with Test Methods D 344 or D 2805. 9. Properties of the Dry Film 9.1 Abrasion Resistance--Abrasion resistance is a mea sure of the ability of a dried film to withstand wear from foot traffic and marring from objects rolled or pulled across the surface. Determine abrasion resistance in accordance with Test Methods D 658 or D 968. 9.2 Elongation--Elongation is a measure of the flexibility of a paint film. Determine elongation in accordance with Test Methods D 1737 or D 522. 9.3 Adhesion--Adhesion is the property of the film that resists removal from the substrate when scuffed or scraped. It is an important property in a floor paint. Determine adhe sion in accordance with Test Method D 2197. 9.4 Resistance to Chemicals--An important property of a floor paint is its ability to resist spotting, softening, or removal when subjected to household chemicals or strong cleaners. Determine resistance to chemicals in accordance with Test Method D 1308. 9.5 Exterior Exposure--If the paint is intended for use on porches, decks, or outside stairways and railings, tests for resistance to exterior exposure may be required and may include the following: 9.5.1 Conducting Exterior Exposures--In conducting ex terior exposures, refer to Practice D 1006 and Classification D 1848. 9.5.2 Wood Panel Description--In establishing exposure performance, use the panels as described in Specification D 358. 9.5.3 Chalking Resistance--Determine the chalkresistance rating by reference to Test Method D 659. 9.5.4 Checking Resistance--Determine the checking re sistance rating by reference to Test Method D 660. 9.5.5 Cracking Resistance--Determine the cracking re sistance rating by reference to Test Method D 661. 9.5.6 Erosion Resistance--Determine the erosion resist ance rating by reference to Test Method D 662. 9.5.7 Flaking Resistance--Determine the flaking resist ance rating by reference to Test Method D 772. 10. Analysis of Paint 10.1 Chemical Analysis--If a specification requires cer tain raw materials or certain components in a given amount then chemical analysis is required to determine whether the specified components are present and in what amounts. Analysis does not necessarily establish paint quality which can also be greatly affected by manufacturing techniques. Most ASTM analytical methods apply to solvent-reducible coatings. However, some of these can be adapted for analysis of water-borne paints. 10.2 Volatile Content--The percent of volatile matter indicates the thinner loss from the film as it dries. This quantity subtracted from 100 % gives the nonvolatile con tent. Determine the volatile content in accordance with Test Method D 2369. 10.3 Pigment Analysis--The analysis of pigment may be required if the product is covered by a specification or if it is 475 DU P050297656 agreed between the purchaser and the seller. Analyze the pigment in accordance with selected test procedures from Methods D 215. 11; Index Terms 11.1 This guide is indexed under the following termsfloor paints/coatings. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement ofsuch rights, are entirely their own responsibility. This standardis subject ro revision atany time by the responsible technical committee and must be reviewed every five years and It not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. [ 1. Scoj j. 1.1 ' | adhesie | and rex film. [ 1.2 ' r sites w laborat for filrt [ N' Test Me j employe 1.3 ' adhesie level, adhesie ment a r N' | the coat the samt S 1.4 1 betwee [ the sut 1.5 ' problei ; user i \ health ! limita, 2. Rei 2.1 D60 Pa D82 TT Te D 17 mi D20 nix 476 `Thes Paint anc Subcomir Currer published 2 Anni 3 Anm ... DU P05 02 97657 Designation: D 3359 - 90 Standard Test Methods for Measuring Adhesion by Tape Test1 This standard is issued under the fixed designation D 3359; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. These methods have been approvedfor use by agencies ofthe Department ofDefense. Consult the DoD Index ofSpecifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. j. Scope U These test methods cover procedures for assessing the adhesion of coating films to metallic substrates by applying and removing pressure-sensitive tape over cuts made in the film. 1.2 Test Method A is primarily intended for use at job sites while Test Method B is more suitable for use in the laboratory. Also, Test Method B is not considered suitable for films thicker than 5 mils (125 (im). N' 1--Subject to agreement between the purchaser and the seller. Test Method B can be used for thicker films if wider spaced cuts are employed. 1.3 These test methods are used to establish whether the adhesion of a coating to a substrate is at a generally adequate level. They do not distinguish between higher levels of adhesion for which more sophisticated methods of measure ment are required. N' 2--It should be recognized that differences in adheiability of the coating surface can affect the results obtained with coatings having the same inherent adhesion. 1.4 In multicoat systems adhesion failure may occur between coats so that the adhesion of the coating system to the substrate is not determined. 1.5 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting3 D 2092 Practices for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Painting2 D2370 Test Method for Tensile Properties of Organic Coatings2 D3330 Test Method for Peel Adhesion of PressureSensitive Tape of 180 Angle4 D4060 Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser2 3. Summary of Test Methods 3.1 Test Method A--An X-cut is made in the film to the substrate, pressure-sensitive tape is applied over the cut and then removed, and adhesion is assessed qualitatively on the 0 to 5 scale. 3.2 Test Method B--A lattice pattern with either six or eleven cuts in each direction is made in the film to the substrate, pressure-sensitive tape is applied over the lattice and then removed, and adhesion is evaluated by comparison with descriptions and illustrations. 4. Significance and Use 4.1 If a coating is to fulfill its function of protecting or decorating a substrate, it must adhere to it for the expected service life. Because surface preparation (or lack of it) has a drastic effect on adhesion of coatings, a test method for evaluating adhesion to different surface treatments or of different coatings to the same treatment is of considerable use in the industry. 4.2 The limitations of all adhesion methods and the specific limitation of this test method to lower levels of adhesion (see 1.3) should be recognized before using it. The intra- and inter-laboratory precision of this test method is similar to other widely-accepted tests for coated substrates (for example, Test Method D2370 and Test Method D 4060), but this is partly the result of it being insensitive to all but large differences in adhesion. The limited scale of 0 to 5 was selected deliberately to avoid a false impression of being sensitive. TEST METHOD A--X-CUT TAPE TEST 5. Apparatus and Materials 5.1 Cutting Tool--Sharp razor blade, scalpel, knife or other cutting devices. It is of particular importance that the 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.23 on Physical Properties of Applied Paint Films. Current edition approved Oct 26, 1990. Published December 1990. Originally published as D 3359 - 74. Last previous edition D 3359 - 87. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 02.05 and 06.06. 4 Annual Book ofASTM Standards, Vol 15.09. 5 Permacel' 99 manufactured by Permacel, New Brunswick; NJ 08903, and available from various Permacel tape distributors, is reported to be suitable for this purpose. The manufacturer of this tape and the manufacturer of the tape used in the interlaboratoiy study3 have advised this subcommittee that the properties of these tapes were changed. Users of it should, therefore, check whether current material gives comparable results to previous supplied material. I DUP0502 97658 D 3359 cutting edges be in good condition. 5.2 Cutting Guide--Steel or other hard metal straightedge to ensure straight cuts. 5.3 Tape-One-inch (25-mm) wide semitransparent pres sure-sensitive tape with an adhesion strength agreed upon by the supplier and the user is needed. Because of the variability in adhesion strength from batch-to-batch and with time, it is essential that tape from the same batch be used when tests are to be run in different laboratories. If this is not possible the test method should be used only for ranking a series of test coatings. 5.4 Rubber Eraser, on the end of a pencil. 5.5 Illumination--A light source is helpful in determining whether the cuts have been made through the film to the substrate. 6. Test Specimens 6.1 When this test method is used in the field, the specimen is the coated structure or article on which the adhesion is to be evaluated. 6.2 For laboratory use apply the materials to be tested to panels of the composition and surface conditions on which it is desired to determine the adhesion. N' 3--Applicable test panel description and surface preparation methods are given in Methods D 609 and Practices D 1730 and D 2092. . N' 4--Coatings should be applied in accordance with Test Methods D 823, or as agreed upon between the purchaser and the seller. No t e 5--If desired or specified, the coated test panels may be subjected to a preliminary exposure such as water immersion, salt spray, or high humidity before conducting the tape test. The conditions and time of exposure will be governed by ultimate coating use or shall be agreed upon between the purchaser and seller. 7. Procedure 7.1 Select an area free of blemishes and mitior surface imperfections. For tests in the field, ensure that the surface is clean and dry. Extremes in temperature or relative humidity may affect the adhesion of the tape or the'coating. 7.2 Make two cuts in the film each about 1.5 in. (40 mm) long that intersect near their middle with a smaller angle of between 30 and 45. When making the incisions, use the straightedge and cut through the coating to the substrate in one steady motion. 7.3 Inspect the incisions for reflection of light from the metal substrate to establish that the coating film has been penetrated. If the substrate has not been reached make another X in a different location. Do not attempt to deepen a previous cut as this may affect adhesion along the incision. 7.4 Remove two complete laps of the pressure-sensitive tape from the roll and discard. Remove an additional length at a steady (that is, not jerked) rate and cut a piece about 3 in. (75 mm) long. 7.5 Place the center of the tape at the intersection of the cuts with the tape running in the same direction as the smaller angles. Smooth the tape into place by finger in the area of the incisions and then rub firmly with the eraser on the end of a pencil. The color under the transparent tape is a useful indication of when good, contact has been made. 7.6 Within 90 30 s of application, remove the tape by seizing the free end and pulling it off rapidly (not jerked):' back upon itself at as close to an angle of 180 as possible. 7.7 Inspect the X-cut area for removal of coating from the substrate or previous coating and rate the adhesion in accordance with the following scale: 5A No peeling or removal, 4A Trace peeling or removal along incisions or at their intersection, 3A Jagged removal along incisions up to Vis in. (1.6 mm) on either side, 2A Jagged removal along most of incisions up to */s in. (3.2 mm) on either side, 1A Removal from most of the area of the X under the tape, and 0A Removal beyond the area of the X. 7.8 Repeat the test in two other locations on each test panel. For large structures make sufficient tests to ensure that the adhesion evaluation is representative of the whole surface. 7.9 After making several cuts examine the cutting edge and, if necessary, remove any flat spots or wire-edge by abrading lightly on a fine oil stone before using again. Discard cutting tools that develop nicks or other defects that tear the film. 8. Report 8.1 Report the number of tests, their mean and range, and for coating systems, where the failure occurred that is, between first coat and substrate, between first and second coat, etc. 8.2 For field tests report the structure or article tested, the location and the environmental conditions at the time of testing. 8.3 . For test panels report the substrate employed, the type of coating, the method of cure, and the environmental conditions at the time of testing. 8.4 If the adhesion strength of the tape has been deter mined in accordance with Test Method D 3330, report the results with the adhesion rating(s). 9. Precision and Bias6 9.1 In an interlaboratory study of this test method in which operators in six laboratories made one adhesion measurement on three panels each of three coatings covering a wide range of adhesion, the within-laboratories standard deviation was found to be 0.33 and the between-laboratories 0.44. Based on these standard deviations, the following criteria should be used forjudging the acceptability of results, at the 95 % confidence level: 9.1.1 Repeatability--Provided adhesion is uniform over a large surface, results obtained by the same operator should be considered suspect if they differ by more than 1 rating unit for two measurements.- 9.1.2 Reproducibility--Two results, each the mean of triplicates, obtained by different operators should be consid ered suspect if they differ by more than 1.5 rating units. 9.2 Bias cannot be established for these test methods. TEST METHOD B--CROSS-CUT TAPE TEST 10. Apparatus and Materials 10.1 Cutting Tool--Sharp razor blade, scalpel, knife'or other cutting device having a cutting edge or edges ang 6 Supporting data arc available from ASTM Headquarters. Request I D01-1008. 478 betwt sever cuttir 10. posec straig 10. meas 10 10 10 10 used area. 11. ' 11 12. 12 spec test i blerr 12 illun 12 inch mak 12 2.0 < apar Test i: thro just edgt wit! i: witl rib! 1 any stoi cen 1 refit beei 1. Rer rate 1 aree goo on indi 1 seiz as c 1 sub maj DUP050297659 eher on d test that 'hole edge S by =ain. that and t is, ond the e of type ntal Ber the in ion -ing ud ies ng Its a aid ing of ;id- or led SR: n [5 and 30 that will make either a single cut or cuts at once. It is of particular importance that the svePg e(jge be in good condition. 2 Cutting Guide--If cuts are made manually (as op t0 a mechanical oarpspnaorranftiutes^) ao estfedeall o <r Aotthliaerr lhioarf/di WmAettoal ,seu ' - or template to ensure straight cuts. 103 Ru*e--Tempered steel rule graduated in 0.3 mm for during individual cuts. 1810 4 Tape, as described in 5.3. 10 5 Rubber Eraser, on the end of a pencil. 10.6 Illumination, as described in 5.5. 10.7 Magnifying Glass--An illuminated magnifier to be ^ while making individual cuts and examining the test area. U Test Specimens 11.1 Test specimens shall be as described in Section 6. 12. Procedure 12.1 Where required or when agreed upon, subject the specimens to a preliminary test before conducting the tape lest (see Note 3). After drying or testing, select an area free of blemishes and minor surface imperfections. 12.2 Place the panel on a firm base and under the illuminated magnifier make parallel cuts as follows: 12.2.1 For coatings having a dry film thickness up to and including 2.0 mils (50 pm) space the cuts 1 mm apart and make eleven cuts unless otherwise agreed upon. 12.2.2 For coatings having a dry film thickness between 2.0 mils (50 pm) and 5 mils (125 pm), space the cuts 2 mm apart and make six cuts. For films thicker than 5 mils use Test Method A. 12.2.3 Make all cuts about 3A in. (20 mm) long. Cut through the film to the substrate in one steady motion using just sufficient pressure on the cutting tool to have the cutting edge reach the substrate. When making successive single cuts with the aid of a guide, place the guide on the uncut area. 12.3 After making the required cuts brush the film lightly with a soft brush or tissue to remove any detached flakes or ribbons of coatings. 12.4 Examine the cutting edge and, if necessary, remove any flat spots or wire-edge by abrading lightly on a fine oil stone. Make the additional number of cuts at 90 to and centered on the original cuts. 12.5 Brush the area as before and inspect the incisions for reflection of light from the substrate. If the metal has not been reached make another grid in a different location. 12.6 Remove two complete laps of tape and discard. Remove an additional length at a steady (that is, not jerked) rate and cut a piece about 3 in. (75 mm) long. 12.7 Place the center of the tape over the grid and in the area of the grid smooth into place by a finger. To ensure good contact with the film rub the tape firmly with the eraser on the end of a pencil. The color under the tape is a useful indiction of when good contact has been made. 12.8 Within 90 30 s of application, remove the tape by seizing the free end and rapidly (not jerked) pulling it off at as close to an angle of 180 as possible. 12.9 Inspect the grid area for removal of coating from the substrate or from a previous coating using the illuminated magnifier. Rate the adhesion in accordance with the fol lowing scale illustrated in Fig. 1: 5B The edges of the cuts are completely smooth; none of the squares of the lattice is detached. 4B Small flakes of the coating are detached at intersections; less than 5 % of the area is affected. 3B Small flakes of the coating are detached along edges and at intersections of cuts. The area affected is 5 to 15 % of the lattice. 2B The coating has flaked along the edges and on parts of the squares. The area affected is 15 to 35 % of the lattice. 1B The coating has flaked along the edges of cuts in large ribbons and whole squares have detached. The area affected is 35 to 65 % of the lattice. 0B Flaking and detachment worse than Grade 1. 12.10 Repeat the test in two other locations on each' test panel. 13. Report 13.1 Report the number of tests, their mean and range, and for coating systems, where the failure occurred, that is, between first coat and substrate, between first and second coat, etc. . 1.3.2 Report the substrate employed, the type of coating and the method of cure. 13.3 If the adhesion strength of the tape has been deter mined in accordance with Test Method D 3330, report the Classification of Adhesion Test Results Classification Surface of cross-cut area from which flaking has occurred. (Example for six paralled cuts! 58 None l 48 4-- T1 ~ 38 2B IB 08 Greater than 65% FIG. 1 Classification of Adhesion Test Results 479 i k [ DUP050297660 D 3359 results with the adhesion rating(s). 14. Precision and Bias6 14.1 On the basis of two interlaboratory tests of this test method in one of which operators in six laboratories made one adhesion measurement on three panels each of three coatings covering a wide range of adhesion and in the other operators in six laboratories made three measurements on two panels each of four different coatings applied over two other coatings, the pooled standard deviations for withinand between-laboratories were found to be 0.37 and 0.7. Based on these standard deviations, the fc Should be used for judging the acceptability 95 % confidence level: 14.1.1 Repeatability--Provided adhesion is uniform oVer a large surface, results obtained by the same operator should be considered suspect if they differ by more than one ratia unit for two measurements. 8 14.1.2 Reproducibility--Two results, each the mean 0{ duplicates or triplicates, obtained by different operators should be considered suspect if they differ by more than two rating units. 14.2 Bias cannot be established for these test methods. 1 [ I I i \ The American Society for Testing and Materials takas no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any sueft patent rights, and the risk of Infringement of such rights, ere entirely their own responsibility. This standard is subject to revision et any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapprdved or withdrawn. Yourcomments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. 480 DU P05 0297661 < Designation: D 3361 - 87 :eria the Standard Practice for over )uld Operating Light- and Water-Exposure Apparatus (Unfiltered ting Open-Flame Carbon-Arc Type) for Testing Paint, Varnish, 1 of tors two Lacquer, and Related Products Using the Dew Cycle1 This standard is issued under the fixed designation D 3361; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice covers the specific variations in test conditions that are applicable when Method 2 in Recom mended Practice G 23 is employed for the exposure of paint and related coatings and materials using the dew cycle with unfiltered open-flame carbon arc. N' 1--Another procedure for exposing these products is covered by Practice D 822 in which specimens are subjected to radiation from the enclosed carbon arc or the filtered open-flame carbon arc. The filters in Practice D 822 remove some of the shorter wavelength ultraviolet radiation not normally received at the earth's surface. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards; D523 Test Method for Specular Gloss2 D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces2 D659 Test Method for Evaluating Degree of Chalking of Exterior Paints2 D660 Test Method for Evaluating Degree of Checking of Exterior Paints2 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints2 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints2 D714 Test Method for Evaluating Degree of Blistering of Paints2 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints2 D822 Practice for Conducting Tests on Paint and Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light- and Water-Exposure Apparatus2 1 This practice is under the jurisdiction of ASTM Committee D-1 on. Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.27 on Accelerated Testing. Current edition approved Nov. 27, 1987, Published January 1988. Originally published as D 3361 - 74. Last previous edition D 3361 - 81, 2 Annual Book ofASTM Standards, Vol 06,01. D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, Lacquer, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D 1212 Methods for Measurement of Wet Film Thickness of Organic Coatings2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 D 1729 Practice for Visual Evaluation of Color Differences of Opaque Materials3 D 1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting4 D 1731 Practices for Preparation of Hot-Dip Aluminum Surfaces for Painting4 D1732 Practices for Preparation of Magnesium Alloy Surfaces for Painting4 D 2092 Practices for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Painting2 D 2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates2 D2616 Test Method for Evaluation of Visual Color Difference with a Gray Scale3 D 4214 Test Methods for Evaluating Degree ofChalking of Exterior Paint Films2 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry5 G23 Practice for Operating Light-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Expo sure of Nonmetallic Materials6 3. Significance and Use 3.1 Organic coatings on exterior exposure are subjected to attack by degrading elements of the weather, particularly ultraviolet light, oxygen, and water. This practice may be used for evaluating the behavior of films exposed in appa ratus that produces ultraviolet radiation, high temperatures, and water condensation on the films. This apparatus is used 3 Annual Book ofASTM Standards, Vol 14.02. 4 Annual Book ofASTM Standards, Vols 02.05 and 06.0!. 5 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 6 Annual Book ofASTM Standards, Vols 06.01, 06.03, and 14.02. DU P0502 97662 # D3361 to make an early materials comparison of the exterior exposure quality of paints. However, light sources, such as the carbon arc, that emit a significant amount of radiation at wavelengths shorter than those in natural sunlight, may cause results that lead to unrealistic evaluations of weath ering properties. 3.2 This test method produces failure of films at a very rapid rate because the test is run without filters. The unfiltered carbon arc produces light that does not exist at the earth's surface. Failure caused by this light may bear no relationship to failures in natural sunlight It is essential to have a control material of known performance of a similar vehicle type in every test. Substrates that have good thermal insulating properties should not be used because sufficient condensation cannot be obtained. 3.3 As no single light exposure apparatus, with or without water, can be specified as a direct simulation of natural exposure, this practice does not imply expressly, or other wise, a specific correlation with outdoor exposure. It has, however, been useful in many instances. 3.4 Since climatic conditions vary with respect to time, geography, and topography, it may be expected that the effects of natural exposure will vary accordingly. All mate rials are not affected equally by the same environment. Results obtained by use of this practice should not be represented as equivalent to those of any outdoor weathering test unless the degree of quantitative correlation has been established for the material in question. 3.5 Variations in results may be expected when operating conditions among similar type instruments vary within accepted limits of this standard procedure. 4. Hazards 4.1 Warning--Never look directly at the carbon arc because ultraviolet radiation can damage the eye. Most carbon arc apparatus machines are equipped with door safety switches, but users of old equipment must be certain to turn the operate switch off before opening the. test chamber door. 4.2 This light source generates ozone and nitrous oxides. Exhaust from the cabinet should be vented to the atmo sphere. 5. Test Specimens 5.1 Unless otherwise agreed upon, choose panels that meet the applicable base panel requirements specified in Test Methods D 609 and Practices D 1730, D 1731, D 1732, or D 2092. Select panel sizes suitable for exhibiting the failure mode to be observed. 5.2 Apply the coatings to flat panels with the base panel material, method of application, coating system, film thick ness, and method of drying consistent with the anticipated end use, or as mutually agreed upon between the producer and the user. 5.3 Unless otherwise agreed upon, coat test panels in accordance with Test Methods D 823 and measure the film thickness in accordance with an appropriate procedure selected from Test Methods D 1005, D 1186, D 1212, or D 1400. Nondestructive methods are preferred because panels so measured do not need to be repaired. 5.4 Unless otherwise specified, before exposing coated panels in the apparatus, condition them at 73.5 3.5F (23 I-5- no refe 2C) and 50 5 % relative humidity for one of the be tests cor following periods in accordance with the type of coating: iccompanie Baked coatings 24 h eference p: Radiation-cured coatings 24 h All other coatings 7 days min j0. Report 6. Apparatus io.l Re 6.1 Type EH Apparatus (open-flame carbon arc), 0f 10.1.1 1 Practice G 23, without filters.7 7. Procedure 7.1 Mount the test specimens vertically both above and below the horizontal center line of the source of radiation. Rotate the specimens from upper to lower rack to provide uniform exposure conditions over their surface. Specimens should be exposed approximately as many hours in the top rack as in the bottom rack, but need not be inverted. 7.2 Base temperature measurement and control on the black panel thermometer unit. Support the panel with the thermometer attached in the top row of the specimen drum or rack in the same manner as the test specimens so that it will be subjected to the same influences. If necessary, read black panel temperatures through the window in the test chamber without opening the door. The black panel temperature shall reach a maximum of 145 9F (63 5C) during the light-on-without-water-spray period of the test cycle and the equilibrium relative humidity of the air in the test chamber shall be 50 5 %. The chamber temperature shall be 90 5F (32 3C) during the light-off-with-water-spiay period of the test and the relative humidity of the air shall be 95 5 %. 7.3 The water from the rack spray shall strike the back of the test specimens so that the only water on the face of the panels is from the dew formation caused by the chilled water on the back of the panels. The temperature of the water shall be 45 4F (7.2 2C). The water should have less than 20 ppm of solids. 7.4 Operate the apparatus on a cycle of 60 min dark with water-back spray and 60 min light without water spray/ 8. Periods of Exposure 8.1 Use one of the following methods to determine the j duration of the exposure under this practice: 8.1.1 A mutually agreed upon specified number of total hours (light and dark hours), 8.1.2 Number of total hours of exposure required to produce a mutually agreed upon amount of change in either j the test specimen or an agreed upon standard sample. 9. Evaluation of Results 9.1 Evaluate conditions of exposed test specimens bj means of one or more of the following standards: Ted Methods D 523; D 610, D 659, D 660, D 661, D 662, D 714, D 772, D 2244, D2616, D4214, and E97 and Practices, D 1729. Select methods in accordance with product requirements. 9.2 Because of possible variations in results as described 7 Apparatus and carbon arcs from the Atlas Electric Devices Co., 41 Ravenswood Ave,, Chicago. [L 60613, have been found suitable for this purpow^ 482 DUP0502 97663 *F(23 of the ng: n c), of D 3361 3.5, no reference should be made to res'ults obtained from tlxe tests conducted in the apparatus using this practice unless accompanied by Section 10 or unless otherwise specified in a reference procedure. j0. Report 10.1 Report the following information: 10.1.1 Type and model of apparatus used and type of carbon arc, 10.1.2 Total hours of test (dark plus light hours), 10.1.3 Operating black-panel temperatures, 10.1.4 Operating relative humidities, 10.1.5 Test specimen preparation, 10.1.6 Results of evaluation tests, and 10.1.7 Identification of standards used for comparative evaluation. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is sub/ect to revision at any time by the responsible technicalcommittee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either torrevision ofthis standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St, Philadelphia, PA 19103. 483 DUP0502 97664 Designation: D 3363 -74 (Reapproved 1989)1 Standard Test Method for Film Hardness by Pencil Test1 This standard is issued under the fixed designation D 3363; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. " N' --Sections 2 and 3 were editorially renumbered in March 1989. 1. Scope 1.1 This test method covers a procedure for rapid, inex pensive determination of the film hardness of an organic coating on a substrate in terms of drawing leads or pencil leads of known hardness. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Summary of Test Method 2.1 A coated panel is placed on a firm horizontal surface. The pencil is held firmly against the film at a 45 angle (point away from the operator) and pushed away from the operator in a `A-in. (6.5-mm) stroke. The process is started with the hardest pencil and continued down the scale of hardness to either of two end points: one, the pencil that will not cut into or gouge the film (pencil hardness), or two, the pencil that will not scratch the film (scratch hardness). 3. Significance and Use 3.1 This test method is especially useful in developmental work and in production control testing in a single laboratory. It should be recognized that the results obtained may vary between different operators and laboratories. Every effort should be made to standardize the hardness of the lead used and the technique followed. If used as a basis for purchase agreement, this test method will achieve maximum precision if a given set of referee pencils be agreed upon between the purchaser and the seller. 4. Apparatus 4.1 A set of calibrated drawing leads (preferred) or equiv alent calibrated wood pencils meeting the following scale of hardness:2 1 This method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.23 on Physical Properties of Applied Paint Films. Current edition approved Oct. 25, 1974. Published November 1974. 1 Pencils from many manufacturers have been and may be used in pencil hardness testing but it was apparent to the test group (D01.53.02) that the leads supplied by two manufacturers were more uniform, and reproducible results could be obtained from batch to batch of leads. These are Microtomic, manufactured by Faber Castell, 551 Spring Place Rd,, Lewisburg,TN 37091, aadTurquoiss-T2375, manufactured by Mohawk, Route #30, Perth Road, Amsterdam, NY 12010. 6B-5B-4B-3B-2B-B-HB-F-H-2H-3H-4H-5H-6H Softer Harder The difference between two adjacent leads shall be consid ered one unit of hardness. 4.2 Mechanical Lead Holder, for drawing leads if used.3 4.3 Mechanical Sharpener, draftsman-type, is helpful for I trimming wood pencils if used.4 4.4 Abrasive Paper, grit No. 400. 5. Test Specimens and Conditions 5.1 Apply the surface coating by appropriate means to a I smooth rigid substrate and cure properly, or use representa- j tive panels cut from coated stock. The panels used, the I curing conditions, and the age of the coating prior to the testJ shall be within the limits agreed upon between the purchaser | and the seller. 5.2 The film thickness of the coating shall be as specified j or as agreed upon between the purchaser and the seller. 5.3 Conduct the test at 77 3.5F (25 2C) and 50 j 5 % relative humidity. 6. Procedure 6.1 For wood pencils, remove approximately 3/i6 to >/ in. j (5 to 6 mm) of wood from the point of each pencil using a I draftsman-type mechanical sharpener, being careful to leave 1 an undisturbed, unmarked, smooth cylinder of lead. Holding the pencil or lead holder (when using drawing leads) at an angle of 90' to the abrasive paper, rub the lead against the paper maintaining an exact angle of 90 to the abrasive paper until a flat, smooth and circular cross section is obtained, free of chips or nicks in the edge of the cross section. The desired edge may be attained by cementing the abrasive paper to a flat motor-driven disk. By supporting the pencil at | 90' to the rotating disk a uniform flat lead end may be| obtained more reproducibly.5 6.2 Place the coated panel on a level, firm, horizontal! surface. Starting with the hardest lead, hold the pencil or lead ! holder firmly with the lead against the film at a 45' angle! (point away from the operator) and push away from thef operator. Exert sufficient uniform pressure downward andl forward either to cut or scratch the film or to crumble the j 3 Turquoise No. 10 is the preferred holder, however, any holder adequately j constructed to eliminate lead slippage may be used. 4 Dexter Super 10 Draftsman Type AI0D Cutter Assembly, manufactured byf Apsco Products, Inc., or equivalent, has been found suitable. | 5 A suitable device for this purpose is available from Gardner Laboratories, Inc., j P. O. Box 5728, Bethesda, Md. j 484 DUP05 02 97665 consid- used.3 pful for ms to a resenta;ed, the the test irehaser pecified ler. id 50 0 V4 in. using a to leave -folding 1 at an 1st the paper ;ained, 1. The irasive lencil at may be rizontal or lead 5 angle om the ird and lble the D 3363 jge of the lead. It is suggested that the length of the stroke 1/4 in. (6.5 mm). 6.3 Repeat the process down the hardness scale until a ncil is found that will not cut through the film to the substrate (either metal or a previous coat) for a distance of at least '/ in. (3 mm) (see 7.1.1). N' 1--The operator must watch closely for cutting into or watching the film. Some finishes contain compounds that may tend to fabricate the film. Checks should be made by close visual inspection and m fingernail feel. N' 2--In conducting the test, ifthe sharp edge ofthe lead is slightly ^pped or crumbled, the lead must be resharpened. 6.4 Continue the process until a pencil is found that will neither cut through nor scratch the surface of the film. Any defacement of the film other than a cut (gouge) is considered a scratch. Record each end point (ifapplicable) for gouge and scratch hardness (see 7.1). N' 3--With some films, the two end points will be identical. 6.5 Make a minimum of two determinations for gouge hardness (6.3) and scratch hardness (6.4) for each pencil of lead. 7. Report 7.1 Report the following information: 7.1.1 The two end points as follows: 7.1.1.1 Gouge Hardness--The hardest pencil that will leave the film uncut for a stroke length of at least Vs in. (3 mm). 7.1.1.2 Scratch Hardness--The hardest pencil that will not rupture or scratch the film. 7.1.2 The make and grade of lead or pencil used, and 7.1.3 Any deviation from standard conditions, including roughness in the finish. 8. Precision 8.1 In an interlaboratory test of this test method with three different films on panels, ten laboratories and opera tors, and repeated by switching leads and panels between laboratories, the within-laboratory standard deviation was found to be 0.52 and the between-laboratory standard deviation was found to be 0.61. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at a 95 % confidence level: 8.1.1 Repeatability--Two results obtained by two opera tors within a laboratory using the same pencils and panels should be considered suspect if they differ by more than one pencil unit on the scale described in 4.1. 8.1.2 Operator Reproducibility--Two results, each the mean of at least two determinations, obtained by operators in different laboratories using the same pencils and panels or different pencils with the same panels should be considered suspect if they differ by more than one pencil unit on the scale described in 4.1. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users ofthis standard are expressly advised that determination of the validity ol any such patent rights, and the risk 0i Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee cn Standards, 1916 Race St., Philadelphia, PA 19103. adequately actured by ones, Inc., 485 DUP050297666 Designation: D 3383 - 79a (Reapproved 1986)1 Standard Guide for Testing Solvent-Reducible Floor Paints1 This standard is issued under the fixed designation D 3383; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. N' --Sections 3 and 4 were renumbered and the title was changed in October 1988. 1. Scope 1.1 This guide covers the selection and use of procedures for testing solvent-reducible floor paints and enamels. The test methods included are listed in Tables 1 and 2. 1.2 This guide covers the testing of ready-mixed finish coats applied by brush or roller on surfaces subjected to traffic, such as floors, decks, platforms, stairs, and adjacent surfaces such as stair risers and railings. . 1.3 Floor paints may be intended for interior use only or may also be suitable for use on exterior surfaces exposed to the weather such as decks, porches, porch steps, and carport floors. Paints intended for both exterior and interior use will require certain test procedures not applicable to paints intended for interior use only. Selection oftest methods must' be governed by the requirements in each individual case, together with agreement between the purchaser and the seller. 2. Referenced Documents 2.1 ASTM Standards: D 16 Terminology of Terms Relating to Paint, Varnish, Lacquer, and Related Products2 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester3 D 154 Guide for Testing Varnishes4 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints5 D 215 Methods of Chemical Analysis of White Linseed Oil Paints4 D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts4 D358 Specification for Wood to Be Used as Panels in Weathering Tests of Coatings4 D 522 Test Method for Mandrel Bend Test of Attached Organic Coatings4 D523 Test Method for Specular Gloss4 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer4 D658 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive4 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D 01.42 on Architectural Finishes. Current edition approved May 25 and Oct. 26, 1979. Published December 1979. Originally published as D 3383-75. Last previous edition D 3383-75. 7 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 3 Annual Book ofASTM Standards, Vols 05.01, 06.01, and 06.03. 4 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.01 and 06.02. D659 Method of Evaluating Degree of Chalking 0f Exterior Paints4 D 660 Test Method for Evaluating Degree of Checking 0f Exterior Paints4 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints4 D 662 Test Method for Evaluating Degree of Erosion of Exterior Paints4 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints4 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels4 D968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive4 D 1006 Practice for Conducting Exterior Exposure Tests of Paints on Wood4 D 1014 Test Method for Conducting Exterior Exposure Tests of Paints on Steel4 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems4 D1308 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes4 D 1471 Test Method for Two-Parameter, 60-deg Specular Gloss6 D1475 Test Method for Density of Paint, Varnish, Lao quer, and Related Products4 D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature4 D 1729 Practice for Visual Evaluation of Color Differences of Opaque Materials7 D1737 Test Method for Elongation of Attached Organic Coatings with Cylindrical Mandrel Apparatus8 D 2197 Test Methods for Adhesion of Organic Coatings by Scrape Adhesion4 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates4 D 2245 Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints9 D 2369 Test Method for Volatile Content of Coatings4 D2371 Test Method for Pigment Content of Solvent- Reducible Paints4 6 Discontinued; see 1975 Annual Book ofASTM Standards, Part 27. 7 Annual Book ofASTM Standards, Vol 14.02. 8 Discontinued; see 1988 Annual Book ofASTM Standards, Vol 06.01. 9 Annual Book ofASTM Standards, Vol 06.03. 486 DUP0502 97667 # D 3383 TABLE 1 List of Test Methods by Properties Test Method Liquid paint properties; Skinning Condition in container Coarse particles and foreign matter Density or weight per gallon Fineness of dispersion Consistency Absorption Flash point Paint application and film formation: Application of brushed film Brushing properties Roller coating properties Drying properties Leveling properties Producing films of uniform thickness Appearance of the dry film: Color differences of opaque materials, instrumental evaluation of Color differences of opaque materials, visual evaluation of Gloss Hiding power Properties of the dry film: Abrasion resistance Elongation (flexibility) Adhesion Resistance to chemicals Exterior exposure Conducting exterior exposures on wood Conducting extenor exposures on steel Wood panel description Chalk resistance Checking resistance Cracking resistance Erosion resistance Flaking resistance Analysis of paint: Chemical analysis Volatile content Pigment content Pigment analysis Identification of vehicle solids Identification cf oils ,r Section 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.3 7.1 7.2 7.3 7.4 7.5 7.6 8.2 8.1 6.3 8.4 9.1 9.2 9.3 9.4 9.5 9.5.1 9.5.1 9.5.2 9.5.3 9.5.4 9.5.5 9.5.6 9.5.7 T0.1 10.2 10.3 10.4 10.5 10.6 ASTM Test Methods D 154 D 185 D1475 D 1210 D 562 D 93 or D 3278 D 1640 D 2801 D 823 D2244 D 1729 D 523, D 1471 D 2805, D 344 D 658,D 988 D1737, D522 D 2197 D1308 D 1006 D 1014 D 358 D 659 D 660 D 661 662 D 772 D 2369 D 2371 D215 D2621 D 2245 Federal Test Method Standard No. 141 3021 3011.1 4091 4184.1 4411.1 4281 4421 2141.1 4321.1 4335 4061.1 2121,2162 6123 4249.1 6101 6221 6303.1 6161.1 6160 2031 6411 6421 6471 6431 6441 4041.1 4021,4022 7261 7501 D2621 Test Method for Infrared Identification of Vehicle Solids from Solvent-Reducible Paints4 D 2801 Test Method for Leveling Characteristics of Paints by Draw-Down Method10 D2805 Test Method for Hiding Power of Paints by Reflectometry4 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus9 E 105 Recommended Practice for Probability Sampling of Materials7 2.2 U.S. Federal Test Methods Standard 141:11 1021 Inspection (General) 2121 Application of Dipped Films 2141.1 Application of Brushed Films 3011.1 Condition in Container 4321.1 Brush Properties 4335 Roller Coating Properties 4421 Absorption Test 3. Definitions 3.1 For definitions of terms used in this guide refer to Definitions D 16. 4. Conditions Affecting Performance of Solvent-Thinned Floor Paints 4.1 Practical requirements and performance of solventthinned floor paints may vary with: 4.1.1 Substrate type, such as type and quality of wood, concrete, metal, or composition flooring. 4.1.2 Substrate condition such as porosity, hardness, smoothness, and degree of cleanliness, or in the case of unpainted concrete, alkalinity. 4.1.3 Environmental conditions such as temperature and humidity at the time of application and during drying. 4.1.4 Substrate Aspects---If construction defects are such that excessive moisture makes its way through the substrate, or if the substrate is in direct contact with damp ground, blistering, flaking, or peeling may result. 10 Discontinued; see 1989 Annual Book ofASTM Standards, Vol 06.01. 11 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, 5. Sampling 5.1 Prior to sampling, the condition of the container should be established since damage to it may cause evapora- 487 DUP050297668 # D 3383 TABLE 2 Alphabetical List of Test Methods Test Methods Abrasion resistance Absorption Adhesion Application of brushed films Brushing properties Chaik resistance Checking resistance Chemical analysis Coarse particles and foreign matter Color differences of opaque materials, instrumental evaluation Color differences of opaque materials, visual evaluation Condition in container Conducting exterior exposures on wood Conducting exterior exposures on steel Consistency Cracking resistance Density or weight per gallon Drying properties Elongation (flexibility) Erosion resistance Exterior exposure Fineness of dispersion Flaking resistance Flash point Gfoss Hiding power Leveling properties Oils, identification of Pigment analysis Pigment content Producing films of uniform thickness Resistance to chemicals Roller coating properties Skinning Vehicle solids, identification of Volatile content Wood panel description Section 9.1 6.7 9.3 7.1 7.2 9.5.3 9.5.4 10.1 6.3 8.1 8.2 6.2 9.5.1 9.5.1 6.6 9.5.6 6.4 7.4 9.2 9.5.6 9.6 6.5 . 9.5.7 6.8 8.3 8.4 7.5 10.6 10.4 10.3 7.6 9.4 7.3 6.1 10.5 10.2 9,5.2 ASTM Test Method D 968 D 2197 D 659 D 660 D 185 D 2244 D 1729 D 1008 D 1014 D562 D661 D 1475 D 1640 D 1737. D 522 - - D 662 D 1210 D772 D 93 or D 3278 DS23, D 1471 D 2805, D 344 D 2801 0 2245 D 215 D 2371 D 823 D 1308 D154 0 2621 D 2369 D 358 Federal Tesl Method Standard No. 141 4421 6303.1 2141.1 4321.1 6411 6421 4091 6123 4249.1 3011.1 6161.1 6160 4281 6471 4181.1 4061.1 6221 6431 4411.1 6441 6101 7501 7261 4021, 4022 2121, 2162 4335 3021 4041.1 2031 tion, skinning, or other undesirable effects in the coating. Determine the condition of the coating in accordance with 6.1 and 6.2. 5.2 Sample in accordance with 4.2.1 of Method 1021 of U.S. Federal Test Method Standard No. 141. Determine the weight per gallon in accordance with Test Method D 1475. Repeat this procedure until successive readings agree within 0.1 lb (45 g) or as agreed upon between the purchaser and the seller. Samples for testing may then be taken. 5.3 Specify the amount of sample, the package sizes, and identification codes to assure a representative sample. A 1-gal (4-L) sample is usually sufficient for the recommended tests, but for guidance in selecting a sampling plan consult Recommended Practice E 105. 6. Liquid Paint Properties 6.1 Skinning--Coatings containing a binder that dries by oxidation may be subject to skin formation in a partially filled can. Since skins are insoluble in the material, they must be removed before use. The referenced test method indicates the tendency of a paint to skin. Examine the original sample for skins, both on the surface and in its mass. On a well-mixed, skin-free portion of the sample, perform a skinning test in accordance with Guide D 154. 6.2 Condition in Container--Thickening, settling, and separation are undesirable and objectionable if a paint cannot be reconditioned and made suitable for application with a reasonable amount of stirring. The referenced method covers procedures for determining changes in properties of paints after storage. Determine the condition in the con tainer in accordance with Method 3011.1 of Federal Test Method Standard No. 141. 6.3 Coarse Particles and Foreign Matter--Paints must be free of coarse particles to form uniform films of good appearance, typical maximum being I weight % of total paint. The specified test with a No. 325 (45-gim) screen gives the percent of these particles in a paint. Determine coarse particles and foreign matter in accordance with Test Methods D 185. 6.4 Density or Weight per Gallon--The density as mea sured by weight per gallon or kilogram per litre is used to assure product uniformity from batch to batch. In the referenced test method, the density is expressed as the weight in pounds avoirdupois of 1 U. S. gal (kilogram/litre) of the paint at a specified temperature. A calibrated weight-pergallon cup is used. Determine density in accordance with Test Method D 1475. 6.5 Fineness ofDispersion--The more finely a pigment is dispersed, the more efficiently it is being used. One method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the material down a calibrated, tapered groove in a hardened steel block with the groove varying in depth from 4 to 0 mils (100 to 0 pm). The point at which continuous groupings of particles or agglom erates, o taken a: micromi better fi sion in i 6.6 C applicat upon. Ii as the lc shear. 1 Method 6.7 A determi porous and pen and the as the absorpti Method 6.8 / requirec Part B, 7. Pain 7.1 , be smo marks. Methoc 7.2 1 means The ter in the a the de general vertical on stai proper) Metho< 7.3 quentl procec teristic proper Methc 7.4 impon stair m result exteric appear or not storagt ance v. 7.5 when i and a labora tics of accord 1 7-6 1 lowing 488 i DUP050297669 3383 jiates, or both, protrude through the surface of the liquid is taken as the fineness reading, Lower readings in mils or micrometres or higher readings in Hegman units indicate better fineness of dispersion. Determine fineness of disper sion in accordance with Test Method D 1210. 6.6 Consistency--Consistency is important, relating to application and flow, and should fall within a range agreed upon. In the referenced test method, consistency is defined as the load in grams required to produce a specified rate of shear. Determine consistency in accordance with Test Method D 562. 6.7 Absorption--The referenced method provides a rapid determination of the relative penetration of the binder into a porous surface. It provides a rough measure of the wetting and penetrating properties of liquid materials. Loss of binder and the resultant change in pigment volume concentration as the film dries, are indicated by the test. Determine absorption in accordance with Method 4421 of Federal Test Method Standard No. 141. 6.8 Flash Point--When the flash point of a material is required for shipping information, use Test Methods D 93, Part B, or D 3278. 7. Paint Application and Film Formation 7.1 Application of Brushed Films--Brushed films should be smooth and free from seeds, color streaking, and brush marks. Test application ofa brushed film in accordance with Method 2141.1 of Federal Test Method Standard No. 141. 7.2 Brushing Properties--The specified method covers a means for determining the brushing properties of coatings. The test is quite subjective; however, someone experienced in the art can produce quite consistent results, particularly in the determination of "drag" qualities. Floor paints are generally applied to horizontal surfaces but evaluation on vertical surfaces may be necessary to determine performance on stair risers, railings, posts, etc. Determine the brushing properties in accordance with Method 4321.1 of Federal Test Method Standard No. 141. 7.3 Roller Coating Properties--Floor enamels are fre quently applied by roller. The referenced method outlines a procedure for making an evaluation of a material's charac teristics when applied by a roller. Determine roller coating properties in accordance with Method 4335 of Federal Test Method Standard No. 141. 7.4 Drying Properties--The drying time of a floor paint is important in determining when a freshly painted floor or stair may be subjected to traffic. Slow drying of the film may result in dust pickup, poor appearance, and, if used on an exterior surface, rain or dew may cause a nonuniform appearance. The test can also be used to determine whether or not the drying properties of the paint have changed during storage in the container. Determine drying time in accord ance with Test Method D 1640. 7.5 Leveling Properties--Leveling is an important factor when uniform surfaces are to be produced, as it affects hiding and appearance. The referenced test method covers the laboratory determination of the relative leveling characteris tics of liquid coatings. Determine leveling characteristics in accordance with Test Method D 2801. 7.6 Producing Films of Uniform Thickness--The fol lowing test method covers the preparation of various films of uniform thickness essential in conducting tests. Prepare films in accordance with Test Methods D 823. 8. Appearance of The Dry Film 8.1 Color Differences of Opaque Materials by Visual Evaluation--Visual comparison of color is fast and often acceptable although numerical values are not obtained. The referenced method covers the spectral, photometric, and geometric characteristics of light source, illuminating and viewing conditions, size of specimens, and general proce dures to be used in the visual evaluation of color differences of opaque materials. Determine color difference in accord ance with Practice D 1729. 8.2 Color Differences of Opaque Materials by Instru mental Evaluation--Color difference between a product and the standard can be measured by instrument. Generally the tolerance is agreed upon between the purchaser and the seller. The referenced method covers the instrumental deter mination of small color differences, observable in daylight illumination, between nonfluorescent, nonmetameric, opaque surfaces such as paint specimens. If metamerism is suspected, visual evaluation (8.1) should be used to verify instrumental results. Conduct instrumental evaluation of color difference in accordance with Method D 2244. 8.3 Gloss--Floor enamels generally have a high initial 60-deg gloss reading when first applied. Determine the specular gloss in accordance with Test Methods D 523 or D 1471. 8.4 Hiding Power (Dry Opacity)--Hiding power is the measure of the ability of a paint to hide the substrate. It is, however, dependent upon uniform film thickness which is influenced by flow and leveling. Test Method D 344 is a practical test in which paint is applied with a brush, film thickness is approximately measured, opacity is evaluated visually as compared to a standard paint, and results are affected by flow and leveling application properties of the paint. Test Method D 2805 is considered to be a more precise and accurate test which does not need a material paint standard. Paint is applied with an applicator bar to minimize the effects of flow and leveling, film thickness is rigorously measured, and opacity is instrumentally evalu ated. Determine hiding power in accordance with Test Methods D 344 or D 2805. 9. Properties of the Dry Film 9.1 Abrasion Resistance--Abrasion resistance is a mea sure of the ability ofa dried film to withstand wear from foot traffic and marring from objects rolled or pulled across the surface. Determine abrasion resistance in accordance with Test Methods D 658 or D 968. 9.2 Elongation--Elongation is a measure of the flexibility of paint films. Determining elongation in accordance with Test Methods D 1737 or D 522. 9.3 Adhesion--Adhesion is the property of the film which resists removal from the substrate when scuffed or scraped. It is an important property in a floor paint. Determine adhe sion in accordance with Test Methods D 2197. 9.4 Resistance to Chemicals--An important property of a floor paint is its ability to resist spotting, softening, or removal when subjected to household chemicals or strong 489 DUP050297670 4f!f # 0 3383 cleaners. Determine resistance to chemicals'in accordance with Test Method D 1308. 9.5 Exterior Exposure--If the paint is intended for use on porches, decks, or outside stairways and railings, tests for resistance to exterior exposure may be required. 9.5.1 Conducting Exterior Exposures--In conducting ex terior exposures, refer to Practice D 1006 or Test Method D 1014. 9.5.2 Wood Panel Description--In establishing exposure performance, use die panels as described in Specification D358. 9.5.3 Chalk Resistance--Determine the chalk-resistance rating by reference to Method D 659. 9.5.4 Checking Resistance--Determine the checking re sistance rating by reference to Test Method D 660. 9.5.5 Cracking Resistance--Determine the cracking re sistance rating by reference to Test Method D 661. 9.5.6 Erosion Resistance--Determine the erosion resist ance rating by reference to Test Method D 662. 9.5.7 Flaking Resistance--Determine the flaking resist ance rating by reference to Test Method D 772. 10. Analysis of Paint 10.1 Chemical Analysis--If a specification requires cer tain raw materials or certain components in a given amount then chemical analysis is required. Chemical analysis deter mines whether the specified components are present and if they are, in what amounts. It does not necessarily establish paint quality which can also be greatly affected by manufao. turing techniques. No single schematic analysis is compre. hensive enough to cover the wide variety of floor enamej composition. 10.2 Volatile Content--The percent of volatile matte, indicates the thinner loss from the film as it dries. This quantity subtracted from 100 % gives the nonvolatile con. tent Determine the volatile content in accordance with Test Method D 2369. 10.3 Pigment Content--Pigment gives the hiding and color and influences many other properties of a coating. Determine the percent pigment in accordance with Test Method D 2371. 10.4 Pigment Analysis--The analysis of pigment maybe required ifthe product is covered by a specification, or if it is agreed between the purchaser and the seller. Analyze the pigment in accordance with selected test procedures from Method D 215 and other appropriate ASTM Test methods. 10.5 Identification of Vehicle Solids--The type of nonvolatile vehicle used in a coating has a great influence on its properties. The referenced test method gives a procedure for identifying the main components of the binder. Determine the identity of the vehicle solids in accordance with Method D 2621. 10.6 Identification of Oils--The composition of the non volatile vehicle can, if desired, be further broken down into the types of oils present. Determine the identity of oils in accordance with Method D 2245. The American Society for Testing and Materials takes noposition respecting the validity ofany patentrights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any tinm by the responsible technical committee and must be tevlmed every live years and ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your wews known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. S 1. prin ligh ratii 2- 1 2 E E C C c 3. 3 tan' ma 4. 4 rat An Pr; spc Th {: Rela DO C 2 1 490 DU PO50297671 tfacPreanel atter This conTest and ting. Test y be it is the rom ads. ivoii its 5 for nine :hod loninto s in Designation: D 3424 - 75 Standard Method of Evaluating the Lightfastness of Printed Matter1 This standard is issued under the fixed designation D 3424; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. j. Scope 1.1 This method covers evaluation of the lightfastness of printed matter. Two methods of exposure, direct to artificial light and under glass to natural light, and three methods of rating the fastness are provided. 5. Test Specimens 5.1 The type and number of test specimens to be used shall be defined in specifications covering the product being tested or shall be mutually agreed upon by the purchaser and the seller. % Referenced Documents 2.1 ASTM Standards: D1729 Practice for Visual Evaluation of Color Differences of Opaque Materials2 D 2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates3 D2616 Test Method for Evaluation of Visual Color Difference With a Gray Scale2 G24 Practice for Conducting Natural Light Exposures Under Glass2 G 25 Practice for Operating Enclosed Carbon-Arc Type Apparatus for Light Exposure of Nonmetallic Materials4 G27 Practice for Operating Xenon-Arc Type Apparatus for Light Exposure of Nonmetallic Materials4 3. Significance 3.1 Lightfastness of printed matter is of particular impor tance in uses such as posters, billboard prints, advertising matter, and display materials generally. 4. Apparatus 4.1 Method A, Exposure to Artificial Light--The appa ratus to be used is described in Section 3 of Practice G 27. An alternative light source is described in Section 3 of Practice G 25. The spectrum of the xenon arc is closer to the spectrum of daylight. 4.2 Method B, Exposure to Natural Light Under Glass-- The apparatus to be used is described in Section 3 of Practice G 24. 1 This method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials, and is the direct responsibility of Subcommittee D01.56 on Printing Inks. Current edition approved July 25, 1975. Published October 1975. 2 Annual Book ofASTM Standards, Vol 14.02. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Discontinued, see 1979 Annual Book ofASTM Standards, Part 41. 6. Procedure 6.1 Mask approximately one quarter of each print with a material opaque to light. Expose the prints for a period mutually agreed upon by the purchaser and the seller to the required conditions. 6.2 After exposure, compare the unexposed portion to the exposed part using one of the following three procedures as agreed upon by the purchaser and the seller: 6.2.1 Visual rating against a control exposed at the same time. 6.2.2 Visual rating using gray scale color chips in accor. dance with Method D 2616. 6.2.3 Instrumental measurement in accordance with Method D 2244. 7. Report 7.1 When a report is required, the designation of the specimen and the description or identification of the method used to prepare the specimen should be included. 7.2 The report will depend upon the procedure used for evaluating the results and should be agreed upon by the purchaser and the seller. 7.2.1 For Procedure 6.2.1, visual rating against a control exposed at the same time, viewing condition should be included as described in Practice D 1729. Report the spec imen as being equal to or having more or less light fastness than the control. 7.2.2 For Procedure 6.2.2, visual rating using gray scale color ships, report information as in Method D 2616. 7.2.3 For Procedure 6.2.3, instrument measurement, re port information as in Method D 2244. 8. Precision 8.1 For precision of the rating method, see Method D 2244 or Method D 2616, where applicable. 491 DUP050297672  D 3424 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprctved or withdrawn. Your comments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. I 1 | t i j ScoPe I 'l.i T1 l for testic { gilJlfllClS* and 2. A | Select ; govcnicc I vidualc: | and the 2. Refer 2.1 A D16 and D93 Clo D 154 D I8f Pas D34c the D 521 Orj D52: D56 Stc D82 Th Te DIO PI' D 12 me D 12 of D 14 qu 'This Related ( DO 1.42 i Currei Publishec 2Anm 3 Ann: * 4 Ann. 5 Ann 6 Ann | DUP050297673 j|Jj^ Designation: D 3425 - 80 (Reapproved 1988)1 Standard Guide for Testing Solvent-Reducible Interior Semigloss Wall and Trim Enamels1 This standard is issued under the fixed designation D 3425; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (s) indicates an editorial change since the last revision or reapproval. 41 N' --Editorial changes were made throughout, including the title, in October 1988. j. Scope This guide covers the selection and use of procedures w testing solvent-reducible interior wall and trim semigloss mantels. The test methods included are listed in Tables 1 .(j 2. All ofthese tests may not be required for each enamel, flection of the test methods to be followed must be ,0verned by experience and the requirements in each indi vidual case, together with agreement between the purchaser and the seller. 2, Referenced Documents 2.1ASTM Standards: 016 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester3 D154 Guide for Testing Varnishes4 0185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints5 0344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Bmshouts4 0522 Test Methods for Mandrel Bend Test of Attached Organic Coatings4 D523 Test Method for Specular Gloss4 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer4 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels4 D1038 Definitions of Terms Relating to Veneer and Plywood6 D1210 Test Method for Fineness of Dispersion tif Pig ment-Vehicle Systems4 D1212 Methods for Measurement of Wet Film Thickness of Organic Coatings4 D1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products4 ' This practice is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials, and is the direct responsibility of Subcommittee DO 1.42 on Architectural Finishes. Current edition approved Aug. 1, 1980. Published December 1980. Originally Published as D 3425 - 75. Last previous edition D 3425 - 79. 1Annual Book ofASTM Standards, Vols 06.01,06.02 and 06.03. 3Annual Book ofASTM Standards, Vols 05.01, 06.0! and 06.03. 1Annual Book ofASTM Standards, Vot 06.01. .................. ......... 'Annual Book ofASTM Standards, Vols 06.01 and 06.02. 6 Annual Book ofASTM Standards, Vol 04.09. D1543 Test Method for Color Permanence of White Architectural Enamels4 D1554 Definitions of Terms Relating to Wood-Base Fiber and Particle Panel Materials6 D1640 Test Methods for Drying, Curing, or Film Forma tion of.Organic Coatings at Room Temperature4 . D1729 Practice for Visual Evaluation of Color Differences of Opaque Materials7 D1737 Test Method for Elongation of Attached Organic Coatings with Cylindrical Mandrel Apparatus8 D2196 Test Methods for Rheological Properties of NonNewtonian Materials by Rotational (Brookfield) Vis cometer4 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates4 D2369 Test Method for Volatile Content of Coatings4 D2371 Test Method for Pigment Content of Solvent- Reducible Paints4 D2697 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings4 D 2698 Method for Determination of the Pigment Content of Solvent-Reducible Paints by High-Speed Centri fuging4 D2801 Test Method for Leveling Characteristics of Paint by Draw-Down Method9 D2805 Test Method for Hiding Power of Paints by Reflectometry4 D 3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus10 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry11 12 E 105 Recommended Practice for Probability Sampling of Materials7 2.2 U. S. Federal Test Methods Standard 141A2 1021 Sampling General 2112 Preparation of Gypsum Wallboard Panels 2131 Application of Sprayed Films 2141 Application of Brushed Films 3011.1 Condition in Container 4203.1 Reducibility and Dilution Stability ' Annual Book ofASTM Standards, Vol 14.02. 8 Discontinued; see 1988 Annual Book ofASTM Standards, Vol 06.01. 8 Discontinued; see 1989 Annual Book ofASTM Standards, Vol 06.01. 10 Annual Book ofASTM Standards, Vol 06.03. 11 Annua! Book ofASTM Standards, Vols 06.01 and 14.02. 12 Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 493 DU PO 5 02 97674 J i, : >> : < # D 3425 TABLE 1 List of Teat Methods by Properties Test Method Section^ ASTM Test Method Federal Test Method Standard No. 141 Liquid enamel properties: Skinning Condition in container Coarse particles and foreign matter Weight per gallon or density Fineness of dispersion Odor Consistency (viscosity) Rheological properties of non-newtonian liquids Dilution stability Absorption Flash point Color compatibility Enamel application and film formation: Application of brushed films Application by roller Application of sprayed films Drying properties Leveling properties Working properties Sag resistance Wet film thickness Producing films of uniform thickness Appearance of dry enamel film: Color difference of opaque materials, visual evaluation Color difference of opaque materials, instrument evaluation Directional reflectance Gloss (60 deg specular) Hiding power Color change of white architectural enamels Properties of dry enamel film: Elongation (flexibility) Washability Analysis of enamel: Chemical analysis Volatile content Pigment content Analysis of pigment Nonvolatile content (volume percent) 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8 6.9 6.10 6.11 6.12 7.1 7.2 7.3 7.4 7.5 7.6 7.7 7.8 7.9 8.1 8.2 8.3 8.4 8.5 8.6 D 154 D 185 D 1475 D1210 D 562 D 2196 3021 3011.1 4091 4184.1 4411.1 4401 4281 D 93, D3278 4203.1 4421 4293 - D1640 D2801 D1212 D 823 2141.1. 4321.1 2112 2131 4061.1- 4541 4494 2121, 2162 D 2244 4249.1 D 1729 6123 6 97 D523 D344, D2805 D 1543 6121 6101 9.1 D1737, 6221 D 522 9.2 6141 10.1 10.2 2369 4041..1 10.3 D 2371 4021, 4022' 10.4 10.5 D2697 4311 4321.1 Brushing Properties 4401 Odor Test 4421 Absorption Test 4494 Sag Test (Multinotch Blade) 4541 Working Properties and Appearance of Dried Film 6141 Washability of Paints 3. Definitions 3.1 For definition of terms used in this guide, refer to Definitions D 16, D 1554, and D 1038. 4. Conditions Affecting Performance of Solvent-Type Inte rior Semigloss Wall and Trim Enamel 4.1 Performance of solvent-reducible interior semigloss wall and trim enamels may vary with: TABLE 2 Alphabetical List of Test Methods Test Method Absorption Analysis of pigment Section 6.10 10.4 ASTM Test Method Fed^T^ Method StandTM No. i4l 4421 ^ j&e we 1475 pd the ' 5.3 5 identifi Application of brushed films 7.1 2141.1 1-gal Application by roller Application of sprayed films Chemical analysis Coarse particles and foreign matter Color change of white architectural enamels Color compatibility Color difference of opaque materials, instrument evaluation 7.2 7.3 10.1 6.3 8.6 6.12 8.2 D 185 D1543 D 2244 ,, ^l.l 2113 2131 tests b g.ecom 4091 6. Li9 6-1 oxidat 6123 filled c Color difference of opaque materials, visual evaluation Condition in container Consistency (viscosity) Dilution stability Directional reflectance Drying properties Elongation (flexibility) Fineness of dispersion Flash point Gloss (60 deg specular) Hiding power 8.1 D 1729 42491 are in: 6.2 6.7 D 562 3011.1 4281 use. T tender 6.9 4203.1 skinni 8.3 E 97 6121 1). Exa 7.4 9.1 D1640 D 1737, 4061.1 6221 and ii D 522 ; sarnpl 6.5 D 1210 4411.1 p 154 6.11 D93, 4293 D3278 8.4 D 523 6101 8.5 D 344, 6.2 sepan after Leveling properties Nonvolatile content (volume percent) Odor Pigment content Producing films of uniform thickness Rheological properties of nonNewtonian liquids Sag resistance Sampling Skinning Volatile content Washability Weight per gallon or density Wet film thickness Working properties D 2805 suitat 7.5 10.5 6.6 D 2801 D 2697 4311 4401 The i chanj 10.3 D 2371. 4021, in th 7.9 D 2698 0 823 4022 2121. 2161 Fedei 6.3 6.8 D 2196 be fr unifc 7.7 5 E 105 4494 0.5 v 6.1 D154 3021 ; 325 ( 10.2 D 2369 4041.1 enan 9.2 6.4 D 1475 6141 4184.1 acco 7.8 D 1212 6.< 7.6 4541 mea to l 4.1.1 Substrate, such as type and quality of drywaft pro' fron plaster, wood, or hardboard. 4.1.2 Condition of substrates--presence of grease, dirt, and mold; also porosity, adhesion, and general condition of proi den (kill previous coating. : A ci 4.1.3 Preparation of previously painted substrates in per cluding detergent cleaning, solvent etching, and sanding. 4.1.4 Type and quality ofprimer or undercoat and time of 6. the drying before topcoating. tape 4.1.5 Environmental conditions, both , general and spe I var cific, at the time ofenamel application and immediately after | whi application. bot 5. Sampling 5.1 The condition of the container prior to sampling should be established since damage to it may cause evapoft* tion, skinning, or other undesirable effects. Determine the condition of the enamel in accordance with 6.1 and 6.2. 5.2 Sample in accordance with Section 4.2.1 of Method 1021 of Federal Test Method Standard No. 141. Determine 494 DUP050297675 D 3425 <leral T9s, Method Standard No. 141 wST-'" 2141.1 4321.] 2112 2131 m weight per gallon in accordance with Test Method p]475. Repeat this procedure until successive readings \fee within 0.1 lb (45 g) or as agreed between the purchaser the seller. Then take samples for testing. 5,3 Specify the amount of sample, the package sizes, and identification codes to assure a representative sample. A I.gal (4-L) sample is usually sufficient for the recommended tests but for guidance in selecting a sample plan consult ^commended Practice E 105. 4091 5123 4249.1 5011.1 1281 1203.1 5121 1061.1 5221 1411.1 1293 >101 311 ,401 021 4022 121, 2161 494 021 ' 041.1 141 184.1 541 ywall, , dirt, ion of tes in ns:ime of d spely after ipling, aporane the i.2. lethod :rmine 4, Liquid Enamel Properties 6.1 Skinning--Enamels containing a binder, that dries by oxidation may be subject to skin formation in a partially jOed can or by diffusion of air into a filled can. Since skins jte insoluble in the enamel, they must be removed before ose. This test in a partially filled container indicates the tendency of an enamel to skin. A typical minimum time for sinning in accordance with the referenced test method is 48 jt. Examine the original sample for skins, both on the surface and in its mass. On a well-mixed, skin-free portion of the sample, perform a skinning test in accordance with Guide' 0154. 6.2 Condition in Container--Thickening, settling, and separation are undesirable and objectionable if an enamel, i after storage, cannot be readily reconditioned and made ! suitable for application with a reasonable amount of stirring, j The referenced method covers procedures for determining j changes in properties after storage. Determine the condition in the container in accordance with Method 3011.1 of Federal Test Method Standard No. 14 L. 6.3 Coarse Particles and Foreign Matter--Enamels must be free of oversize particles and foreign matter to form a uniform film of good appearance, a typical maximum being 0.5 weight % of total enamel. The specified test with a No. 325 (45-pm) screen gives the percent of these particles in an enamel. Determine coarse particles and foreign matter in ; accordance with Test Method D 185. 6.4 Weight per Gallon--The density of an enamel as measured by weight per gallon (or kilograms per litre) is used to assure product uniformity from batch to batch and provides a check against the theoretical weight calculated ; from the formula. The referenced test method gives a procedure for measurement of the density ofan enamel. The density is expressed as weight in pounds of 1 U.S. gal (kilograms per litre) of the enamel at a specified temperature. | A calibrated weight-per-gallon cup is used. Determine weight | per gallon in accordance with Test Method D 1475. 6.5 Fineness of Dispersion--One method for measuring ; the degree of dispersion is to draw the enamel down in a tapered groove in a hardened steel block with the groove varying in depth from 4 to 0 mils (100 to 0 pm). The point at which continuous groupings of particles or agglomerates, or both, protrude through the surface of the wet film is taken as the fineness reading. Lower readings in mils or micrometres ; or higher readings in Hegman units indicate better disper- ! don. A typical fineness of dispersion requirement is a j leading of 1.0 mil (25 pm) or 6 Hegman for interior j semigloss wall and trim enamels. Determine fineness of i dispersion in accordance with Test Method D 1210, 6.6 Odor--Some solvent combinations produce obnox` bus odors, particularly when painting indoors with inade- s quate ventilation and under advene temperature-humidity conditions. Test for odor in accordance with Method 4401 of Federal Test Method Standard No. 141. 6.7 Consistency--Enamels of a given type should fall within a consistency range agreed upon. In the referenced test method, consistency is defined as the load in grams required to produce a specified rate of shear. Enamels for professional painters are usually formulated at a higher consistency range than consumer enamels. A typical range is 75 to 90-Krebs unit (KU) foi consumer enamels and 90 to 100 KU for professional painter enamels. Determine the consistency of the product in accordance with Test Method D 562. 6.8 Rheological Properties of Non-Newtonian Liquids-- Rheological properties are related to the application and flow properties of the liquid coating. The referenced test method covers the determination of the rheological properties of an enamel and is particularly suited for use with enamels that display thixotropic characteristics. In fact, viscosity under varying conditions of time and rotational speed of the spindle is measured. Determine the rheological properties in accordance with Test Method D 2196. 6.9 Dilution Stability--The diluent suggested for reduc tion should be readily incorporated into the enamel without excessive stirring or shaking. This, test is a measure of the stability of an enamel that has been reduced to a desired viscosity, for example, for spray application. Determine dilution stability in accordance with Method 4203 of Federal Test Method Standard No. 141. 6.10 Absorption--The referenced method provides a rapid means for measuring the relative penetration of the binder into a porous surface. It provides a rough measure of the wetting and penetrating quality of liquid materials. Lass of binder and the resultant change in pigment volume concentration, as the film dries, are indicated by this test. Determine the absorption in accordance with Method 4421 of Federal Test Method Standard No. 141. 6.11 Flash Point--Organic solvents used in enamels have characteristic temperatures at which they will support com bustion. This temperature is known as the flash point. It is often used for danger classification in shipment by common carriers. It is also used to determine conditions of storage to meet fire regulations and also the safety requirements of the Occupational Safety and Health Act (OSHA). Determine the flash point in accordance with Test Methods D93 or D 3278. . 6.12 Color Compatibility--If tinting colors are not ade quately compatible with enamel tint base, lighter, darker, or nonuniform shades of color will develop. Tintability of white bases with colorants of standardized tinting strength is a trade requirement. The test method shall be agreed upon between the purchaser and the seller. An ASTM test method is now being developed. 7. Enamel Application and Film Formation 7.1 Application by Brush--Brushed films should be smooth and free of seeds and on vertical surfaces should show no sagging, color streaking, or excessive brush marks. Test application-of brushed films in accordance with Method 2141.1 of Federal Test Method Standard No. 141. 7.2 Application by Roller--Walls are frequently painted 495 i i DU PO50297676  D3425 with rollers that produce slight stipple effects. Test roller coating properties in accordance with Method 2112 of Federal Test Method Standard No. 141. 7.3 Application by Spray--Interior paints and enamels are sometimes applied by spray. Both air and airless spray are used in commercial work. Test in accordance with Method 2131 of Federal Test Method Standard No. 141. 7.4 Drying Properties--The drying time of an enamel is determined by the composition of the enamel and by atmospheric conditions during drying. Insufficient drying may result in dirt pickup causing a poor appearance. Typical drying times are >A to 2-h set-to-touch and 18-h dry-hard: The test can also be used to determine whether the enamel has lost its drying properties during storage or whether drier was included in the product at the time of manufacture. Determine the drying time in accordance with Test Methods D 1640. 7.5 Leveling Properties--Leveling is a factor in hiding and appearance of wail and trim enamels. The referenced test method covers the laboratory determination of the relative leveling characteristics of liquid coatings. Determine leveling property in accordance with Test Method D 2801. 7.6 Working Properties--Working properties of an enamel are generally compared to a standard or described by requirement in the product specification. Test working properties in accordance with Method 4541 of Federal Test Method Standard No. 141. 7.7 Sag Resistance--Some enamels sag and form curtains before the film sets. Test for sag resistance in accordance with Method 4494 of Federal Test Method Standard No. 141. 7.8 Wet Film Thickness--Measurement of wet film thickness is useful in calculating spreading capacity or adjusting application to an agreed square feet per gallon (or square metres per litre). Determine wet film thickness in accordance with Method D 1212. 7.9 Producing Films of Uniform Thickness--The fol lowing test method covers the preparation of enamel films of uniform thickness essential in conducting various tests. Prepare films in accordance with Test Method D 823. Determine daylight directional reflectance in accords, with Test Method E 97. 8.4 Glass (60-deg Specular)--Semigloss enamels are >JS ticularly sensitive to enamel hold-out of primers and ""vlv coats. Low or uneven gloss readings are indicative of TM defect. Interior semigloss enamels after drying 48 h typically in the range from 40 to 70 when applied to g_ Gloss measurements taken after 7 days are more indicate of the final gloss of the dried film. Determine the speci gloss in accordance with Test Method D 523. 8.5 Hiding Power (Dry Opacity)--Hiding power is measure of the ability of a paint to hide the substrate, however, dependent upon uniform film thickness which influenced by flow and leveling. Test Method D 344 j|s practical test in which paint is applied with a brush, thickness is approximately measured, opacity is evaluate! visually as compared to a standard paint, and results affected by flow and leveling application properties of 4. paint Test Method D 2805 is considered to be a mil precise and accurate test which does not need a mate paint standard. Paint is applied with an applicator minimize the effects of flow and leveling, film thickness!! rigorously measured, and opacity is instrumentally ev; _ ated. Determine hiding power in accordance with Methods D 344 or D 2805. 8.6 Color Change of White Architectural Enamels--Cojf permanence is an important requirement in interior semigloss enamels. Lack of permanence is usually caused'M after-yellowing. Determine color change in accordance wM Test Method D 1543. IL 9. Properties of Dry Enamel Film jP 9.1 Elongation (Flexibility)--Elongation is a measured flexibility of an enamel film. Determine elongation accordance with Test Method D 1737 or D 522. 9.2 Washability--Washability is an important propel of semigloss enamels in service. It is determined from gloW and reflectance measurements before and after removal || stains. Determine washability in accordance with Methof 6141 of Federal Test Method Standard No. 141. | 8. Appearance of Dry Enamel Film 8.1 Color Difference of Opaque Materials by Visual Eval uation--Visual comparison of color is fast and often accept able although numerical values are not obtained. The referenced practice covers the illuminating and viewing condition to be used in the visual evaluation of color differences. Determine color difference in accordance with Practice D 1729. 8.2 Color Difference of Opaque Materials by Instrument Evaluation--Color difference between a product and the standard can be measured by instrument. Generally the tolerance is agreed upon between the purchaser and the seller, and may also be required if a production specification is involved. Determine the color difference in accordance with Method D 2244. 8.3 Directional Reflectance--This property is a measure of light reflected from the surfaee ofthe enamel. It usually is assigned a value in specifications for white and pastel shades. A typical minimum reflectance value is 86 for white. 10. Analysis of Enamel 10.1 Chemical Analysis--If a specification requires' tain raw materials or certain components in given amoui then analysis is required. Chemical analysis is primatil$| measure of uniformity. It does not necessarily establish i quality which can also be greatly affected by manufactu techniques. No single schematic analysis is comprehensi^l enough to cover the wide variety of semigloss wall and triS enamels. <j 10.2 Volatile Content--The percent of volatile ma indicates the thinner loss from the film as it dries. Deter volatile content of the paint in accordance with Test MetliS D 2369. ' 4 10.3 Pigment Content--Pigment gives the hiding color and influences many other properties of the enamel Determine percent pigment in accordance with Test Methiff D 2371. 10.4 Analysis of Pigment--The analysis of pigment mil be required if the enamel is covered by a specification or ifj| is agreed between the purchaser and the seller. Deter 496 DUP0502 97677 rdance re par. underof this h are 3 glass, licative secular is the e. It is, hich is 14 is a It, film aluated fits are of the i more laterial bar to '-ness is evaluh Test -Color r white asedby ce with D 3425 analysis of pigment in accordance with selected ASTM test methods. 10.5 Nonvolatile Content (Volume Percent)--Nonvolatile content volume percent is a useful figure in calculating coverage or spreading capacity per gallon (or litre) at a specified dry film thickness. Determine nonvolatile content volume percent of the paint in accordance with Test Method D 2697. TheAmerican Society for Testing and Materials takas no position respecting the validity of any patentrights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Your comments are Invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the resfionsible technical committee, which you may attend. If you fee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standerde, 1916 Race St,, Philadelphia, PA 19103. sure of ion in roperty n gloss oval of Tetbod ;s cerlount, irily a h paint during hensive id trim matter .ermine Method ng and mantel. Method nt may < or if h 497 DU P050297678 Designation: D 3450 - 90 7. Reager Standard Test Method for 7.1 Put used in ai Washability Properties of Interior Architectural Coatings1 that all re Committe This standard is issued under the fixed designation D 3450; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. ical Socie grades me reagent is lessening 1. Scope 1.1 This test method covers the determination of the relative ease of removing soilant discolorations from the dried film of an interior coating by washing with either an abrasive or nonabrasive cleaner. 1.2 This test method is limited to coatings having aCIE-Y reflectance of 60 % or more, as measured in accordance with placed on a glass plate in a washability machine and the fil^ is washed with either an abrasive or nonabrasive scrub medium for 100 cycles. The panel is rinsed and dried and the reflectance in the stained area is read [Rfj- The ratio of the reflectance, R2/Ru is a measure of the degree to which the soilant has been removed. 7.2 Pu, ence to v conformii 7.3 Bit 7.4 Sp> 7.5 Mt 7.6 So, Test Method E 97. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 562 Test Method for Consistency of Paints Using the Stormer Viscometer2 D1193 Specification for Reagent Water3 D 1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems2 E 70 Test Method for pH of Aqueous Solutions with the 5. Significance and Use 5.1 Interior architectural paints are often discolored by dirt and other soilant materials. This test method covers the relative ease and completeness of removal of a specific soilant from such a surface by scrubbing. The greater the ease of soil removal with a minimum of film erosion, the greater the useful service life is expected to be. 5.2 Results obtained by this test method do not neces sarily correlate with all types of soilants. 5.3 Semigloss finishes generally require only the nonabrasive type cleaner for good soilant removal, whereas flat paints may require the abrasive type. 6. Apparatus i t c 7.6.1 I of 7 (0.5 with Tesi 7.7 Sc 7.7.1 ; Wate Hydr Deter Triso Aceti Prese Glass Electrode4 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry5 3. Terminology 3.1 Description of Term Specific to This Standard: 3.1.1 soilant--a discoloring substance that clings to the surface of a coating, whose dispersed color component is not in solution and therefore does not penetrate into the film. 3.1.1.1 Discussion--Soilant differs from stain in that the colorant of a stain is in solution, and therefore, can penetrate into the film. 6.1 Washability Tester,6 also referred to as washability machine. 6.1.1 Accessory Apparatus: 6.1.1.1 Glass Plate, measured to fit, 177/s by 6V2 by 'A in. {454 by 165 by 6.3 mm). 6.1.1.2 Stainless Steel Pan. 6.1.1.3 "C" Clamps. 6.1.1.4 Scale, standard. 6.1.1.5 White Blotter. 6.2 U-Shaped Film Caster,7 having both a 7-mil (0.18- mm) clearance by 132 mm width and a 10-mil (0.25-mm) clearance by 138 mm width. 6.3 Film Applicator, 3 in. (76 mm) width with 3-mil 7.7.2 . Wate Hydi Amr Det, Tris Silic Ace' Pres x Vary with a Stor (76-p.m) clearance. 4. Summary of Test Method 4.1 The test material is applied to a black plastic panel and allowed to dry for 7 days. The reflectance of the film is measured (R{) and then a soilant consisting of carbon black dispersed in mineral oil is applied on the film. The panel is 6.4 Suction Plate for drawdowns (large size).8 6.5 45, 0 Reflectometer, with green filter, as specified in Test Method E 97. 6.6 Balance, with 0.1-g scale graduation. 6.7 Fineness of Dispersion Gage, as specified in Test Method D 1210. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.42 on Architectural Finishes. Current edition approved August 31, 1990. Published November 1990. Originally published as D 3450 - 75. Last previous edition D 3450 - 86. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annua! Book ofASTM Standards, Vol 06.03. 4 Annua/ Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 6 Model AG 8100, available from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910, and Model "D" available from Paul N. Gardner Company, Inc., 316 N. E. First St, Pompano Beach, FL 33060 have been found suitable for this purpose. Other straight-line washability testers may be adapted to meet the requirements of this method. See RR DO 1-1065. 7 The Dow film caster has been found satisfactory for this purpose and is available from BYK-Gardner. 8 Available from BYK-Gardner. An equivalent may be used. 9 "Reagi ical Soc., V the Amcrif Joseph Ros Pharmacop '"Lenei 165 by 0. Ho-Ho-Ku 11 Spon; 38 mm) mi General Iv measuring >2 Labo are availab may be usi 13 Print Ridgefield may be usi 498 DUPO 50297679 1 0 3450 i the filrjj ve scrub 3 and the .io of the 'hich the >lored by overs the specific r the ease ie greater at necesthe nonereas flat ishability by `A in. il (0.1825-mm) th 3-mil 7. Reagents and Materials 7.1 Purity ofReagents--Reagent grade chemicals shall be uSed in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.9 Other gjades may he used, provided it is first ascertained that the feagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 7.2 Purity of Water--Unless otherwise indicated, refer ence to water shall be understood to mean reagent water eonforming to Type IV of Specification D 1193. 7.3 Black Plastic Panels.10 1A Sponge and Holder.11 7.5 Masking Tape. 7.6 Soilant Medium,12 consisting of the following: grams Mineral oil, USP heavy Odorless mineral spirits Carbon black13 60 32 8 100 7.6.1 Mix components and disperse to a Hegman fineness of 7 (0.5 mils or 13 pm) or when measured in accordance with Test Method D 1210. 7.7 Scrub Media (Note 1). 7.7.1 Nonabrasive Medium12 consisting of the following: grams Water Hydroxyethyl cellulose14 Detergent15 Trisodium phosphate, anhydrous Acetic acid glacial Preservative16 89.64 2.0 4.0 4.0 0.3-8 0.1 TOOS 7.7.2 Abrasive Medium12, consisting of the following: grams Water Hydroxyethyl cellulose14 Ammonium hydroxide 28 % Detergent15 Trisodium phosphate, anhydrous Silica17 Acetic acid, glacial Preservative16 49.4 c 0.8 -- 2.0 2.0 45.0 . 0.727 0.1 100.0 A Vary to achieve a final consistency of 165 to 220 g (75 to 85 Krebs Units) with a Stormer Viscometer in accordance with Test Method D 562. ecified in in Test Laboratory, Ie from Paul 33060 have sters may be pose and is 9 "Reagent Chemicals, American Chemical Society Specifications.'' Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States I Pharmacopeia." i 10 Leneta, P-121-10N dull black plastic panels 6ft by 17 in. by 10 mils (432 by 165 by 0.25 mm) in size, obtainable from the Leneta Co., P.O. Box 86, Ho-Ho-Kus, NJ are suitable for this purpose. An equivalent may be used. 11 Sponge is a cellulosic type, coarse pore grade, 3ft by 3 by 1 ft in. (95 by 76 by 38 mm) meeting Federal Spec. L-S-626, Type II; available also from O'Cel-O Div., General Mills, Inc., 305 Sawyer Ave., Tonawanda, NY 14150. Brass holder j measuring 3% by 3 by 1 in. (95 by 76 by 25.4 mm). | 12 Laboratory standardized stain and scrub media have been found suitable and tre available from the Leneta Co., P.O. Box 86, Ho-Ho-Kus, NJ. An equivalent may be used. l3Printex U Beads, obtainable from DeGussa Coip., 65 Challenger Road, Ridgefield Park, NJ 07660, has been found suitable for this purpose. An equivalent | may be used. B Vary to achieve a final pH from 9.5 to 10.0 in accordance with Test Method E 70. c Vary to achieve a final consistency of 475 to 600 g (110 to 120 Krebs Units) with the Stormer Viscometer in accordance with Test Method D 562. Vary to achieve a final pH of 9.5 to 10.0 in accordance with Test Method E70. 7.8 Slowly add the hydroxethyl cellulose to the water while stirring mechanically. Stir until uniform and then slowly add 2 to 3 drops of 28 % ammonium hydroxide solution while mixing and continue mixing until the solution turns clear. In the order shown, add the other ingredients separately, stirring continuously. Be sure each item is uni formly dispersed before adding the next one. Add the silica slowly to ensure uniform dispersion. Finally, add the pre servative and adjust the pH with glacial acetic acid. N' 1--When a referee test is made, prepare fresh medium or use standardized scrub medium11 from a previously unopened container that is no more than 1 year old. 8. Preparation of Apparatus 8.1 Washability Machine--The washability machine should be leveled before use and operated at 37 1 cpm; each cycle consisting of a complete forward and reverse stroke. Adjust tautness of the cables with a spring scale to approximately 5 lb. 8.2 Sponge and Holder--Add sufficient weight to the holder in the form of lead sheets or other flat weights to give a combined weight of 1500 g, including the dry sponge. N !' 2--Check the compression of the damp sponge under the 1500-g weight to ensure that the holder does not drag along the panel and tear the film. 9. Procedure 9.1 Clean the top of the glass plate (or preferably the suction plate) and both sides of the black plastic panel to be sure they are free of specks. Place the black panel on the plate and tape one end to the plate. Smooth the panel along the plate to ensure a close fit. 9.2 Stir the test material thoroughly and strain to remove all skins and particles. Draw down the material on the panel, starting from the taped end of the panel. For latex paints, the 10-mil (0.25-mm) side of the applicate will generally be satisfactory, whereas the 7-mil (0.18-mm) side can be used for solvent-based coatings. However, the film thickness of paint to be applied may be varied as mutually agreed upon between the purchaser and the seller. The rate of application should be fairly slow, 3 to 4 s from end to end, to prevent 14 Hydroxyethyl cellulose having a molar substitution (MS) value from 1.8 to 2.5 and a viscosity ofa 2 % solution in the range from 4400 to 6500 cps. Cellosize QP-4400 is available from Union Carbide Corp., P.O. Box 8720, South Charleston, WV 25303 and Natrosol 250M, available from Aqualon Co., 2711 Centerville Rd., Wilmington, DE 19850 have been found suitable for this purpose. 15 Octyl phenoxy polyethoxyetharioL as represented by Triton X-100, obtain able from Rohm & Haas Co., 2 Executive Campus, Suite 320, Cherry Hill, NJ 08002, has been found satisfactory for this purpose. An equivalent may be used. 16 1,3,5-triethyl hexahydro-sym-triazine (Vancide TH), obtainable from R. T. Vanderbilt Co., 30 Winfield St., Norwalk, CT 06855, has been found satisfactory. An equivalent may be used. 17 Silica No. 22, obtainable from Whittaker, Clark and Daniels. Inc., 100 Church St., New York, NY 10007, has been found satisfactory for this purpose. This silica is an amorphous grade of 99+ % silicon dioxide. Average particle size is 2.95 pm with 92 % being less than 40 pm. Surface area is 7600 cm2/g, and will give a pH from 6.8 to 7.2 in reagent water. An equivalent may be used. 499 r r DUPO 502 97680 D 3450 pinholes or holidays in the film. Air dry in a horizontal position for 7 days in a room preferably maintained at 73.5 3.5F (23 2C) and 50 5 % relative humidity, or under conditions mutually agreeable to the purchaser and the seller. 9.3 On the last day of drying, measure the directional reflectance (green filter) of a portion of the panel in accordance with Test Method E 97. Record this value as R 9.4 After reading the reflectance, use the applicator with the 3-mil (76-p.m) clearance to draw down a film of soilant medium perpendicular to the coating film and in the area where the reflectance was measured. Permit the stained panel to dry for 16 to 24 h under the same drying conditions specified in 9,2. 9.5 Clean the glass surface on which the test panel is to be mounted and also the back of the test panel. Attach the test panel to the glass plate and place the mounted test panel, coated side up, in the pan. Clamp the assembly securely to the pan with the "C" clamps, centering the pan so that the sponge boat can move lengthwise on the panel. 9.6 Remove the sponge from the holder and soak it in reagent water at room temperature. Remove the sponge and squeeze repeatedly with one hand until no more water drips from the sponge. Replace the sponge in the holder and pour 15 1 mL of water on the exposed face of the sponge. Stir the scrub medium and spread uniformly across the face of the sponge 10.0 0.1 g of nonabrasive scrub medium. (Use a spatula if necessary, when applying the abrasive scrub medium, to apply uniformly over the sponge.) 9.7 Attach the sponge holder, with the sponge and cleaner face down, to the cables of the washability machine. Add 5 mL of water on each side of the holder in the path of the sponge. Start the motor and allow the sponge to travel 25 cycles at the rate of 37 1 cpm. Ensure that the sponge and holder are level during the run, otherwise uneven wear will occur on the test panel. At the end of 25 cycles, stop the machine, remove the sponge, clean in running water, sqeeze dry, and resoak in water. Wipe off excess stain outside the test area. Repeat the procedure starting in 9.6 with "remove the sponge and squeeze it repeatedly........" for an additional 25 cycles. Repeat the 25-cycle procedure for a total of 100 cycles, each time trying to start and stop the sponge outside the stained area of the panel. 9.8 Remove the test panel from the pan, rinse with running tap water, gently moving the palm of the hand ovj the path of the sponge to remove clinging particles of scrub medium. Blot the panel and then allow to dry at room temperature. After the panel has dried thoroughly, wipe off excess stain outside the test area and measure reflectance m the soiled and washed area of the panel. Record as R2. 9.9 Repeat the test on a second panel and, for each calculate the reflectance recovery in percent as (RJR,} v 100. 9.10 If the mean reflectance recovery for the two panels is less than 96 %, repeat the test on another set of panels using the abrasive scrub medium specified in 7.7.2 and report the results with both mediums. 10. Report 10.1 Report the mean of the two determinations and the type of scrub medium used. 10.2 Report any deviations from the standard procedure. 10.3 Note if erosion occurred in the soiled area. 11. Precision and Bias 11.1 On the basis of an interlaboratory study in which operators in six laboratories tested six coatings, including solvent and water-based systems, and covering a range of pigment volume concentrations (PVC's), the following cri teria should be used for judging the acceptability of the results at the 95 % confidence level: 11.1.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 1.5 % in reflectance recovery with the abrasive cleaner and 9 % in reflectance recovery with the nonabrasive cleaner. 11.1.2 Reproducibility--Two results, each the mean oftwo measurements, obtained by operators in different labo ratories should be considered suspect if they differ by more than 6 % in reflectance recovery with the abrasive cleaner and 25 % with the nonabrasive cleaner. 11.2 Bias--The concept of bias is not applicable to this test method. ! 12. Keywords 12.1 soilant resistance; washability The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standardor for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. 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SpUE * ('/; qoEo j 3<' 30UB Jjo a<jiA (Qooi 'x 9*Uos ji J8 pa tyttAV 3! Polymeric Powder Properties: Particle size and distribution Multiple sieve and analysis i || # D3451 TABLE 1 List of Test Methods Section 8 8.1 ASTM method D1921 Gravelometer Color, pigmented coatings Visual Section 24 25 25.2 ASTM method D 3170 D 1535 89Z.6Z0S0dna zos TO'Ol PA 'spjoptms msvp Hs pmiuy z, JO'80 PA 'spjvpums nusvfo 3foog jomuv n 10'90 PA 'spjvpims' rusvp ya ivnuuy 8861 ax `.psnuuuoosia 01 ; -!pn)M put? ssAipppB pue `si0j[y `siuaxaSid < ' <u o o KqB i -aaaaS qoxqM. `Suxjjssoinjaqj > 3TisB[doxiiiaqj jsqire `jsmXjod { S> ' > > sspipred pspiAtp /Jpng--xapmod Suijvoo Z'P IF ssppjBd uosMioq psddEJi ire sqi Snipnpui auoj rapMod | m {BuajBin ' > smtqoA jnm J3d ' <--Ansusp yjnq \ 'p saopiuijaQ y poxjpsds sswusqjo ssspra q 91 Sutuoiitpaoo jape `Xiipxmnq SAntipj % g T 0 PUB 3,,Z + t IB poB (iqSpms pajip jou) iq3q pasrqjip m apexu sq ipqs sissj qy I' SJtl30I3Jmb3^ [BJ3U30 ^majs^s HD 3H uisn Ag spafqo JO siopo aqi Sai;ndrao;) > > poqpw 80 3 ^saso&mg Suqssx Joj S3A3IS qioi3-3JiA\ > > uoijBogpads n 3 vlS3I sdBX Aq noxssqpv 8uunsB3jv > > spoqjapv issx 6SG ^sgmjBOO jo aouBjsisa-g Suiddno > > poqppj jsax 0I (3 3 z|SJ3pMOX 0 SnqBoo jo s 3' >3 3 aSpg > > poqiajM JS3X L96ZO uo sSup.B03 S< ' > 1 > souBjstsay < < o q uuojqig > > poqjajM jsax 08ZCI d pjoeduq) tiopBUUojsQ pidE-g jo spajjg aqj 0; sSutjBoo " S' < jo aauBisxsag > > poqjsjAj jsax P6LZ (3 ^SSUIJECQ OTireiJO UO SupjBqxaAO jo payg sqi Smuiuuajsci > > s o x < "' > > frfCI j.saqsxuig < ' &< J aouBjsxsa-a juaSiajoa Joj sopoBjg SPZZO ,,3upioBJ3 ap/CQ iBxmaqx-XjtptaitiH JQJ sojBJisqns oqjBjsjM pauxug uo saqsiuxg > > poqjapj isax gpzzd ,sajBuxpJ003 JQpo pajnsBSjM AqBjuauinjjsuj uioij sEorajsjjia Jopo jo uoijBjnopo > > poqjajAj issx PPZZO j.spxxpoxg psiBp-g ptre `jsnboBq `qsrciJBA `jurej Suijsax > > spnBj pais pazniBApo paiBAxssBd -udjq paddxa-PH J uoxjBJBdajg > > poqjapj Jsax i0Za ^uoisaqpy adBjog q s 3> ' 3 o x' S> jo uoxsaqpy > > poqjajq isax 161Z a (^< > < ' > > > saoBjing pais (pszra -' > ' ) paiBOQ-Durz jo uoqBJBdajg > > saoxpgjg Z60ZO ,,sjanb3B3 jo aauBisxsa^ iuug > > poqiaiq isax 16030 nspuaiBjAt axisBid JO (StSiClBUV 3A3ts) 3ZIS sptVBd > > poqpjv IS3X 1361 a , ponsBix JO guqdaiBS > > sarpBJg 868! 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For thermosetting mate- pals, a chemical reaction, either condensation or addition, gjso takes place. This fused film has the uniformity, color, toughness, and other properties associated with protective 3nd decorative coatings. 4.4 fluidity--the ability of a powder to move freely, uniformly, and continuously (somewhat like a liquid) when subjected to certain conditions of pressure, temperature, and velocity of a carrier gas. 4.5 gel time--interval required at a given temperature for 3 powder to be transformed from a dry solid to a gel-like state. '* 4.6 particle size--average diameter of an object having irregular boundaries that can be described in an artificial way js having a diameter. 4.7 particle-size distribution--arrangement of particle size measurements on a powder in groups of specified diameters. 4.8 pourability--the ability of a powder to flow uniformly or to be continuously poured from a container at a steady rate. 4.9 powder coatings--coatings which are protective or decorative, or both, formed by the application of a coating powder (4.2) to a substrate and fused into a continuous film by the application of heat or radiant energy. 4.10 storage stability--the ability of a powder to maintain uniform physical and chemical properties after being sub jected to specified storage conditions. 4.11 volatile content--the quantity expressed as weight percent of the powder which is lost under specified condi tions of temperatures and time. 4.12 cloud chamber technique--method of moving a charged or uncharged object through a charged or uncharged cloud of powder in an enclosed chamber. 4.13 electrostatic deposition--technique of moving and charging powder so that it is deposited onto an oppositely charged substrate by one of the following methods. 4.13.1 fluidized bed technique--method of moving a grounded object over or through an oppositely charged fluidized powder. 4.13.2 spray technique--method of spraying and charging powder so that it is deposited onto an oppositely charged substrate. 4.14 nonelectrostatic deposition--technique of moving powder onto a substrate which may be heated above the fusion point of the powdered material. 4.14.1 spray technique--method of spraying powder onto a substrate which may be heated above the fusion point of the powdered material. 4.14.2 fluidized bed technique--method of dipping a hot object into a container holding the powder suspended in a gas stream so that it resembles a fluid and allowing the powder to melt onto the object being coated. 4.14.3 flame spread technique--method of applying powder using a compressed gas and melting the powder in a flame before the powder impinges on the surface. 5. Sampling 5.1 Sample the powder in accordance with Practice D 1898. 5.2 Prepare specimens as required for the specific tests on the coating. 6. Equipment 6.1 Use the equipment as specified in each method of test. 7. Conditions Affecting Polymeric Powder or Powder Coat ings, or Both 7.1 Practical requirements and performance of powder and powder coating may vary with: 7.1.1 Substrate Type--Ferrous, nonferrous types, plastic, or elastomeric. 7.1.2 Substrate Weathering--Weathering of the substrate will probably adversely affect the performance. 7.1.3 The type, quality, and suitability of the metal treatment or primer used under the powder coating and the time before coating application. 7.1.4 Application conditions. 7.1.5 Contaminants on the surface of the substrate. 7.1.6 Damage to container, size of container, storage time, excessive temperature, and temperature fluctuations which may cause settling, caking, or chemical change. POLYMERIC POWDER PROPERTIES 8. Particle Size and Distribution 8.1 Multiple Sieve Analysis: 8.1.1 This method employs multiple sieves to determine particle sizes and their distribution. Standard 200-mm(8-in.) diameter sieves and a mechanical shaker are used. A representative quantity of the sample is sifted through a series of sieves and the amount retained on each sieve is weighed and calculated as percent of the total specimen. 8.1.2 Apparatus: 8.1.2.1 Sieves--Half-height sieves, 200 mm (8 in.) in diameter, conforming to the requirements of Specification E 11. A selection of sieves encompassing the expected range of particle sizes together with a cover and a bottom pan are required. 8.1.2.2 Mechanical Sieve Shaker with Automatic Time Switch13--The mechanical sieve-shaking device shall be ca pable of imparting uniform rotary motion and a tapping action at the rate of 150 10 taps/min. 8.1.2.3 Balance--A laboratory balance with a minimum capacity of500 g sensitive to 0.1 g, for weighing the specimen and the residues retained on the sieves. 8.1.3 Procedure: 8.1.3.1 If the residues are not to be transferred for weighing, weigh each of the selected sieves and the bottom pan to 0.1 g. Nest the desired sieves in order of diminishing openings with the coarsest sieve on top and the pan on the bottom. 13 Ro-Tap Sieve Shaker has been found suitable for this purpose and is available from W. S. Tyler Co., Cleveland, Ohio 44114. An equivalent may be used. 503 DU P05 0297684 D 3451 8 13.2 Weigh out a 100 0.1-g specimen and transfer it to the top sieve of the stack. N' i--if necessary this test may be made on a specimen of any size from 50 to 200 g. The weight of specimen used shall be stated in the report. 8.1.3.3 Place the cover on the top sieve, and place the stack in the mechanical sieve shaker. Operate the shaker for 10 min 15 s. 8.1.3.4 After shaking, carefully separate the stack of sieves, beginning at the top, and weigh the quantity of material retained on each sieve and that contained in the pan to 0.1 g. This may be accomplished either by transferring the fractions to the balance or by weighing the sieve or pan and its contents, and subtracting the tare weight from the total. If the material is transferred to the balance, carefully brush the sieve on both sides to ensure that adhering particles are transferred. 8.1.3.5 Calculate the percent in each fraction as follows: % = {R/S) x 100 where: R = residue weight, g, and S = specimen weight, g. N' 2--Ordinarily there is a small loss of dust as indicated by the cumulative total weight being less than 100 %. If this loss is not over 2 %, the amount reported through the finest sieve shall be increased until the total of all portions of the sample equals 100%. If the cumulative total is less than 98 %, repeat the test. 8.1.4 Report--The report shall include the following: 8.1.4.1 Complete identification of the sample, 8.1.4.2 Specimen weight, 8.1.4.3 Percent of material retained on each sieve, 8.1.4.4 If required, the total cumulative percent of mate rial retained on each sieve and in the pan, 8.1.4.5 Temperature, and 8.1.4.6 Relative humidity. 8.2 Vacuum Sieve Analysis: 8.2.1 Summary ofMethod: 8.2.1.1 In this method sieving is accomplished by aerody namics so that there is no reduction in particle size and absolutely no wear on the sieves. 8.2.1.2 The housing holds a standard 200-mm (8-in.) sieve and a transparent sieve cover. A slit nozzle rotates slowly below the sieve. An air current, produced by a standard vacuum cleaner-type device, is blown upwards through a hollow shaft and the slit nozzle to the sieve, where it clears the screen. The particles thus suspended in air between the sieve and the sieve cover are separated as the air current circulates. The line materials are blown through the sieve and into a filter bag, while the coarse materials remain on top of the sieve. A manometer indicates the vacuum inside the housing. 8.2.2 Apparatus: 8.2.2.1 Sieves--As described in 8.1.2.1 and transparent sieve cover. 8.2.2.2 Vacuum Sieve Apparatus--A vacuum sieving device14 capable of maintaining inside the housing a vacuum of 5 0.5 in. (127 12.7 mm) of water as measured by a manometer. The slit nozzle which rotates below the sieve shall revolve at a speed of 25 2 rpm. 8.2.2.3 Balance--See8.1.2.3. 8.2.3 Procedure: 8.2.3.1 If the residues are not to be transferred for weighing, weigh each of the selected sieves to 0.1 g. 5.2.3.2 Weigh out a 100 + 0.1 g specimen and transfer it to one of the sieves. N' 3--If necessary, this test may be made on a specimen of any size from 10 to 50 g. The weight of specimen used shall be stated in the report. For small sieve openings, I to 10 g is recommended. 8.2.3.3 Place the transparent cover on the sieve and place the sieve in position on the vacuum sieving apparatus. Operate the sieving apparatus for 5 min 15 s at a vacuum of 5 0.5 in. (127 12.7 mm) of water. 8.2.3.4 Remove the sieve and cover from the apparatus and weigh the quantity of material retained on the sieve and adhering to the cover to the nearest 0.1 g. This may be accomplished either by transferring the retained material to the balance or by weighing the sieve, cover, and contents, and subtracting the tare weight from the total. If the material is transferred to the balance carefully brush the sieve on both sides, and removed all powder from the cover to ensure that all adhering particles are transferred. 8.2.3.5 Repeat the procedure for each sieve used. 8.2.4 Calculate the percent retained on each sieve as follows: % -= (R/S) x 100 : I i ! I 1 where: R -- residue weight, g, and 5 = specimen weight, g. 8.2.5 Report--The report shall include the following: 8.2.5.1 Complete identification of the sample, 8.2.5.2 Specimen weight, 8.2.5.3 Percent of material retained on each sieve, 8.2.5.4 Temperature, and 8.2.5.5 Relative humidity. 8.3 Sonic Sifter Analysis: 8.3.1 Summary ofMethod: 8.3.1.1 In the sonic sifter, the sieves are stationary and agitation is imparted to the particles by an oscillating column of air. Sieve wear and particle attrition are minimal. 8.3.1.2 The sonic sifter consists of a sieving chamber, a diaphragm at the top vibrating at 60 Hz, and a motor with the necessary controls. The amplitude of vibration is adjust able to the nature of the specimen. 8.3.2 Apparatus: 8.3.2.1 Sieves--See 8.1.2.1. 8.3.2.2 Sonic Sifter--A sonic sieving deviceis utilizing a diaphragm vibrating at 60 Hz with controls to adjust the sift amplitude and the pulse amplitude. 8.3.2.3 Balance--An analytical balance with a minimum capacity of 150 g sensitive to 1 mg for weighing the specimen and the residues retained on the sieves^ 8.3.3 Procedure: : \ i | S j 14 Alpine Air Jet Sieve, Model 200, has been found suitable for this purpose and is available from Alpine American Corp., Michigan Drive, Natick, Mass. 01760. An equivalent may be used. 15 Model L3P Sonic Sifter has been found suitable for this purpose and is available from ATM Corp., P.0 Box 2405, Milwaukee, Wise. 53214. An equivalent may be used. 8.3 8.3 top, i top si 8.3 cham ampl: 8.3 the c< perce NO' the we 8.3 8.3 8.3 8.3 8.3 8.3 8.4 8.4 8.4 meast partic using an el modu ture, tional 8.4. by soi a filte select' fractii 8.4. volun diamt 8.4 8.4 using 8.4 requi the s: size r; 8.4. partic round 8.4. 8.4. 8.4. 8.4. shall 1 intenc 16 M, Model 1 from Cc may be 17 Th Nuclepc 504 A DUP050297685 0 3451 d by a e sieve ed for nsfer it i of any d in the i place aratus. acuum jaratus ve and aay be irial to ntents, laterial n both re that eve as ng: y and >lumn ber, a jt with adjust- izing a the sift limum ;cimen se and is *214. An \ ' 8.3.3.1 Weigh and record the weight of each sieve, and of jjje collar, cover, and fines collector. 8.3.3.2 Weigh out a 2.5 0.001-g specimen. 8.3.3.3 Stack the sieves in descending order, coarsest on top, finest on the bottom, and transfer the specimen to the top sieve. 8.3.3.4 Insert the sieve stack assembly in the sieve Camber and lock. Set the sift amplitude at 3 and the pulse amplitude at 10. Operate the sifter for 3 min 15 s. 8.33.5 Weigh each sieve, the fines collector, cover, and the collar, subtract the tare weight for each, and calculate the percent retained on each sieve. N' 4--Include any material adhering to the cover and the collar in pie weights for the top sieve. 8.3.4 Report--The report shall include the following: 83.4.1 Complete identification of the sample,' 83.4.2 Specimen weight, 8.3.43 Percent of material retained on each sieve, 83.4.4 Temperature, and 83.4.5 Relative humidity. 8.4 Electronic Counting Analysis: 8.4.1 Summary ofMethod: \ 8.4.1.1 This method, one of several found valuable for the measurement of particle size, covers the determination ofthe particle size distribution of powder coatings (0.6 to 80.0 pm) using the electronic particle counter.16 This instrument uses an electric current path of small dimensions which is modulated by individual particle passage through an aper ture, and produces individual pulses of amplitude propor tional to the particle volume. 8.4.1.2 The powder is carefully dispersed ultrasonically or by some other appropriate method and a portion is added to a filtered electrolyte. Particle counts are obtained at several selected particle size levels and converted to relative weight fractions assuming constant particle density. 8.4.13 The instrument response is essentially to particle volume (liquid displacement); therefore equivalent spherical diameter is commonly used to express the particle size. 8.4.2 Apparatus: 8.4.2.1 Electronic Particle Counter,16 detecting particles using electric current through a liquid resistor. 8.4.2.2 Aperture Tube, 200-gm diameter. The diameter required is dependent upon the particle size distribution of the sample. Generally any given tube will cover a particle size range from 2 to 40 % of its aperture diameter. 8.4.23 Beaker, 250 to 500-ml, capable of maintaining all particles uniformly in suspension (for example, baffled or round bottom). 8.4.2.4 Ultrasonic Agitator. | 8.4.2.5 Membrane Filtering Device, 0.45-pm filters.17 | 8.4.3 Reagents: j 8.43.1 Purity of Reagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, where such specifications are available.18 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 8.43.2 Purity of Water--Unless otherwise indicated, ref erences to water shall be understood to mean reagent water conforming to Type IT of Specification D 1193. 8.4.33 Dispersing Medium--5 % solution of octyl phenoxy polyethoxyethanol19 in reagent water. 5.4.3.4 Electrolyte--Dissolve 10.0 g of reagent grade so dium chloride (NaCl) in 1000 ml of reagent water, add some bacteriacide such as 70 mg of sodium trichlorophenate then filter twice through the membrane (8.4.2.5). 8.43.5 Wash Water--Reagent water filtered twice. 8.4.4 Procedure: 8.4.4.1 Precalibrate the aperture and electrolyte combina tion following the manufacturer's instruction manual. N' 5--Calibration should be carried out using a lycopodium of microspheres suspension of IS.04-p.m diameter with the half-count procedure as given in the instruction manual. It is necessary to have mutual agreement on monosized system diameters for interlaboratory comparisons. 8.4.4.2 Cone and quarter the sample until a specimen of convenient size is obtained. 8.4.43 Disperse the specimen by adding dispersing me dium from the eye-dropper. Use gentle spatulation until a pasty consistency is obtained. Pick up a small portion of this mixture (about 0.1 ml more or less depending on the particle size of the powder) on a small spatula and rinse with wash water into a 25-ml beaker containing 5 ml of dispersing medium. Place the beaker in the ultrasonic agitator for 30 s and then rinse into 200 ml of electrolyte in the 250 to 500-ml beaker. Fill the beaker to capacity and place in the counting position of the counter stand. 8.4.4.4 Fill the aperture tube with electrolyte. Check the aperture for blockage and clear with a brush if necessary. Set the instrument controls for the smallest particle appropriate for the aperture in use. Typical instrument settings are shown in Figs. 1, 2, or 3'. 8.4.4.5 Take three cumulative counts with 500-pi volume manometer and calculate the mean, which should be be tween 2700 and 5000. If it is not, adjust the particle concentration until it is. If more powder is added, it must be treated the same as the original specimen, except it may be rinsed directly into the beaker after ultrasonic agitation. If the suspension needs dilution, drain some of the suspension through a clean glass tube while agitating and then refill the beaker with electrolyte. 8.4.4.6 Set the instrument controls for normal accumula tion of differential data. Typical instrument settings are shown in Figs. I, 2, and 3. Take three counts at each size level for averaging. 16 Models ZB with M2 accessory. Model B with Model M accessory. Model T, Model TA, and Model TAII have been suitable for this purpose and are available from Coulter Electronics, Inc,, 590 W. 20 St., Hialeah,. FL 3301ft An equivalent may be used. 17 The membrane filters may be Millipore, Gelman, Genera] Electric, Nuclepore, Selas Flotronics metal type, or their equivalent. (i 18 "Reagent Chemicals, American Chemical Society Specifications," Am. Chemical Soc.; Washington, t)C. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin. D. Van Nostrand Co., Inc., New York, NY, and the "United States.fharmacopeia."- 19 Triton X-100`has been found suitable for this purpose and is available from Rohm and Haas Co., Independence Square, Philadelphia, PA. An equivalent may be used. 505 DUP05 02 97686 # 0 3451 Sample----Aperture 0 Diameter Aperture Resistance.. 20 20 INDUSTRIAL Model ."B" or "Z11 DATA AND WEIGHT CONVERSION raoaei "M" or ,fM2" Converter .Electrolyte. f_ Volume. 500 Ml Gain nc JL_Control _L Gattb. Matching .Switch__ 1CK- ( Modoi-^`Pr 128L Model 8 k nifmM Triton X-100 ^f*ailolhrannHo.vniL tL~14 1/3> j-x, A=1/2 for is.Q4Ma_i0pe3r.0. -7--4--.-0- Maa3- RELATIVE VOLUME VALUES k- t.-I-A ,2ilWL RELATIVE &n V Wt. 80.6 20 20 40.3 20 20 20 1/2 20 1/2 1/2 20 1/2 1/4 20 1/4 1/4 20 1/4 1/8 20 1/8 1/8 10 20 l/a 1/8 1/2 1/4 1/8 1/16 1/32 1/64 12 10.08 5 1/8 1/8 1/121 13 9 6AMC VAUU S 4221007 N' ---Typical setting for smallest particle {B.4.4.4) but upper threshold must be turned to full counterclockwise position for cumulative count in 8.4.4.S. FIG. 1 Model "B" or "Z" Typical Worksheet 8.4.5 Precautions: 8.4.5.1 Check the aperture for blockage at the end ofeach count. If blocked clear the aperture with the brush and retake the count. 8.4.5.2 Adjust the sample stand stirrer motor speed to furnish sufficient agitation to maintain a uniform particle suspension but below air bubble generation speeds. 8.4.5.3 Before each analysis flush all the surfaces coming in contact with the specimen. Use clean wash water and wash bottle. 8.4.6 Treatment ofResult: 8.4.6.1 The values obtained in 8.4.4.6 represent relative volume ofthe particles between two particle size levels. They may be plotted directly on semilog graph paper as a histogram (see Fig. 4). 8.4.6.2 The values obtained in 8.4.4.6 may be added cumulatively. All of these cumulative values may then be normalized to 100 % and a cumulative volume percent curve drawn (see Fig. 4). 8.4.6.3 Relative volume and relative weight are inter changeable if a constant density of the particle system is assumed. Therefore, the curves in 8.4.6.1 and 8.4.6.2 can be interpreted as weight histogram and weight percent curves. 9. Package Stability 9.1 Glass Vial Method: 9.1.1 Apparatus: 9.1.1.1 Aluminum-Foil Disk. 9.1.1.2 Steel Shot. 9.1.1.3 Glass Vial, 4-oz (120-ml), approximately 40-mm inside diameter. 9.1.1.4 Balance, sensitive to 0.1 mg. 9.1.1.5 Oven, maintained at 50 0.5C. 9.1.1.6 Particle Size Determination Apparatus--See Sec tion 8. 9.1.1.7 Powder Coating Application Apparatus--See Sec tion 19.2. 9.1.2 Procedure: 9.1.2.1 Weigh 45 g or as otherwise specified of powder into the glass vial. Place an aluminum-foil disk on top of the powder. Prepare a sufficient number of glass vials for determining sprayability and other properties that may be tested. 9.1.2.2 Weigh ! 50 g of steel shot onto the disk and seal the vial. Place the vial in an oven maintained at 50 0.5'C unless otherwise specified. 506 No t C 9.1 failu: sellei (a 8). (b Cc spec pow . ' DUP050297687 SAMPLE ELECTROLYTE Isoton EQUIPMENT SERIAL ORGANIZATION OPERATOR DATE t- D 3451 Model T Worksheet O.SPERSANT Xriton X_10Q 5% Aper. Die. 200 Ser. No. CALIBRATION DATA Part, Dla. w [A A 18.04 7 Co to 344 FOR MODEL T 1A CALI B. A 3.2 241 APERTURE DIA Geometric Mean ^43 Volume ^i3 Diameter Channel (W) .00575 ,0115 .0231 .0462 .0925 .1551 .3702 .7405 1.451 2.962 5.924 11.85 23.70 47.39 94.78 189.6 379.1 758.3 1516. 3033. 066. 12.13* 103 24.27 * 103 43.54 * 103 97.18* 103 194.4 x ID3 388.7 x 103 777.4 * 103 1.5S5* 106 3.109 x 10 6.219 * 106 12.44 * 106 24.38 * 106 49.75* 106 99.50 x 106 . 199.0* 106 393.0 x 10 798.0* 106 .004091 .008181 .01636 .03272 .06545 .1309 .2618 .5236 1.047 2.094 4.189 8.378 16.76 33.51 67.02 134.0 268.1 536.2 1072. 2145. 4289. 8579. 17.16* 103 34.31 x 103 68.63 x 103 137.3* !03 274.5 x 103 549,0 x 103 1.098* 10 2.196 X 10 4.392 x 10 8.784 x 10B 17.57 xIO8 38.14* 108 70.27 x 108 140.6 x 1082B1.1 x 10 562.2 x 108 .198 .250 .316 .397 .500 .630 .794 1.00 1.26 t.59 2.00 2.52 3.17 4.00 5.04 6.35 8.00 10.0B 12.7 16.0 20.2 25.4 32.0 40.3 50.8 64.0 80.6 101.6 128. 161. 203. 256. 322. 406. ' 512. 645. 612. 1024. 13* 12 11 10 9 8 7 6 5 4 3 2 i Q 21"*-".! Fo Mo*IT SAMPLE DATA N' --Typical settings for smallest particle (8.4.4.4). Cumulative count data readout required for (B.4.4.5). FIG. 2 Model "1 '' Typical Worksheet AltlOOB 9.1.2.3 At 24-h intervals perform the following tests until I failure or as agreed upon between the purchaser and the seller. (a) Particle size and particle size distribution (see Section 8). (b) Gel time (see Section 14). (c) Spray a panel of the powder coating and bake as specified. Compare with a panel prepared with unheated powder. : (d) If there is noticeable caking, test for pourability by Method D 1895. 9.1.3 Report: 9.1.3.1 Duration of test, 9.1.3.2 Particle size distribution before and after testing, 9.1.3.3 Gel time before and after testing, 9.1.3.4 General appearance of panels coated with aged and unaged powders, and 9.1.3.5 Degree of caking. 507 s DUP050297688 SAMPLE ELECTROLYTE rso(.on EQUIPMENT ORGANIZATION OPERATOR SERIAL OATE # D 3451 Model a & TAiiWorksheet OfSPERSANT Aper. id. Ser. No. 200 x.100 5% CALIBRATION DATA Pert. Oia. 18.04 w t [A A 9 4.0 167. Geometric .00575 .0115 .0231 .0462 .0925 .1851 .3702 .7405 1.481 2562 5.924 11.85 23.70 47.39 94.78 189.6 379.1 758.3 1516. 3033. 6066. 12.13x103 24.27 x 103 48.54 x 103 97.18 x 103 194.4 x 103 388.7 x 103 777.4 x 103 1.655 x 10s 3.109 x 10s 6.219 x 10 12.44x10 24.88 X 10B 49.75 x 10 99.50 x 10 199.0 x 106 398.0 x 10 7960 x 10 tIA 4. 0 CALI8. A 139 APERTURE DIA. 200 1 Volume /43 DiameterJU Channel {W) .004091 .008181 .01636 .03272 .06545 .1309 .2618 .5236 1.047 2.094 4.189 8.378 16.76 33.51 67.02 134.0 268.1 536.2 1072. 2145. 42B9. 8579. 17.16 x TO3 34.31 x 103 68.63 x 103 137.3 x 103 274.5 x 103 549.0 x 103 1.09B X 10 2.196 x 10s 4.392 x 10 8.784 x 106 17.57 x 10 35.14 x 10 70.27 x 10 140.6 x 10 281.1 x 106 562.2 X 10 .198 .250 .315 .397 .500 .630 .794 1.00 1.26 1.59 2.00 2.52 3.17 4.00 3* 5.04 6.35 8.00 10.0B t2.7 16.0 20.2 25.4 32.0 40.3 50.8 64.0 80.6 101.6 4 5 6 7 8 9 10 11 12 13 14 1*7 . 1A 128. 161. 203. 256. 322. 406. 512. 645. 312. 1024. ... SAMPLE DATA - N' --Typical setting for smallest particle (8.4.4.4). Cumulative count data readout required tor (8.4.4.S). FIG. 3 Model TA and TAII Typical Worksheet 427J008 9.2 Package Stability (Moisture): 9.2.1 Open-Dish Method--Weigh 10 g of powder into an uncovered 50-mm diameter aluminum dish and place at 40 3C, 95 + 5 % relative humidity, or conditions as agreed upon between the purchaser and the seller. Check for caking or change of gel time after 48 h. 10. Pourability 10.1 Test for pourability in accordance with Test Method D 1895. .. 11. Fluidity 11.1 A method is under consideration. 12. Nonvolatile-Content- ... - - , 12.1 Apparatus: 12.1.1 Analytical Balance, sensitive to 0.1 mg. 508 0S4Xiz*rioh OPEtATM (QVfPMEHT urn L_ tea 12.1 deep. 12.2 12.2 by dif specifi 12.: the be 12.2 60 betwe' and w DUP050297689 k \ #- D 3451 Cumulative Value Plot ......... Differential Value Plot FIG. 4 Size Distribution Curve on Semilog Paper 12.1.2 Aluminum Dishes, 60 mm in diameter and 17 mm deep. 12.2 Procedure: 12.2.1 Weigh two aluminum dishes to 0.1 mg. and weigh by difference two specimens of 1.9 to 2.1 g or as otherwise specified of coating powder into them. 12.2.2 By gentle tilting spread the powder uniformly.over the bottom of the dishes. 12.2.3 Heat the dishes and contents in an oven for 2 h at 60 2C or at 100 2C or at the temperature specified between the purchaser and the seller. Cool in a desiccator and weigh. 12.3 Calculation--Calculate the nonvolatile content as follows: Nonvolatile content, weight % = (C - A) 100/5 where: `; . A = weight of dish, g, S = weight of specimen, g, and C = weight of dish and contents after heating, g. 13. Volatile Content at Baking or Fusion Temperature ....... 13.1 Use the apparatus and procedure given in Section 12 but heat the specimen at the normal baking temperature and time unless otherwise specified. 13.2 Calculate the percent volatile matter by subtracting the nonvolatile content from 100. 14. Gel Time or Stroke Curve (for Thermosetting Powders Only) 14.1 Apparatus: 14.1.1 Hot Plate, suitable for use at 200C. 14.1.2 Stop Watch or Electric Timer, 0.1 s interval. 14.1.3 Wooden Tongue Depressor, 6 by 1 in. (150 by 25 mm) or Wooden Splints, 6 by 'A in. (150 by 6 mm). 14.1.4 Aluminum Foil. 14.1.5 Analytic Balance. 14.1.6 Pyrometer, suitable for use at 200C. 14.2 Procedure: 14.2.1 Measure 0.5 0.1 g of powder. 14.2.2 Cover the hot plate with aluminum foil or use a non-silicon mold release lubricant. Set the heat to 190 1C or as agreed between the purchaser and seller, and check with the pyrometer. N' 6--A shroud may be required to prevent air circulation from cooling the hot plate. 14.2.3 Drop the powder specimen on the foil and start the 509 DU P 0502 97690 D 3451 COVER FOAM flUUBE VACUUM CLEANER BAG SAC CHAMBERManiiftctui*i! In* 132 mm plnimttd 9 < . FIG. 5 Powder Flowmeter timer. Rub the powder with the edge of the tongue depressor in 1 in. (25 mm) diameter circular strokes. Continue this motion with slight pressure until a solid gel is produced as found by lifting the depressor at least 2 in. (50 mm) from the hot plate. If the material produces a continuous filament from the plate to the depressor it has not gelled. 14.2.4 Stop the timer when the strand breaks readily. Repeat the test with a fresh specimen. Calculate and report the mean gel time. 15. Melting Point Determination 15.1 Apparatus: 15.1.1 Kofler Hot Bench,20 hot bench agreed upon be tween the purchaser and the seller. 15.1.2 Calibrating Test Substances: Azobenzene Naphthalene Benzoic acid Melting Point, 68 I 80 0.5 122 1 15.1.3 Paint Brush, stiff bristle, `/2-in. (12.7-mm). 15.2 Procedure: t20 Kofler hot bench has been found suitable and is available from Reichert Co., Vienna, Austria. An equivalent may be used. 15.2.1 Calibrate the apparatus as follows. Allow 60 min for the warm up of the heating bar. Sprinkle a calibrating substance having the closest melting point to that of the powder on the heating bar. Observe the sharp division between solid and liquid. Place the pointer between these two divisions. Slide the reading device to the melting point of the calibrating substance. 15.2.2 Sprinkle the specimen over the heating bar in a uniform manner. Observe the specimen after 1 to 2 min. Brush the material towards the lower temperature and note the location where particles of powder adhere to the bar when brushed lightly. Place-the pointer at this point. Read the temperature and report in degrees Celsius. N' 7--Powder will fuse and "set" on the hot bar. Remove the powder quickly and thoroughly before the setting occurs. Do not use abrasives to clean the bar. 16. Viscosity Measurement for Molten Powder Coatings by Weissenberg Rheogoniometer 16.1 Summary of Method--This method covers the de termination of the viscosity of powder coatings at baking temperatures and consists simply of preheating the cone and plate ofa:Weissenberg rheogoniometerrpouring an-adfequate* sample of powder onto fee plate, closing the apparatus and recording revolutions pec minute and the corresponding . I 1 l tI\ 2 Ii'> \ stead: 16. least temp* surfac 16.: 16manu measi s. Afte to bri agreec few dt 16.: tionin suffici plate suffici until t by th reache 16.3 torque Cautio be exc again.; severa readin. two be Newto 16.3 shear r torsior eviden viscosi on the this. St rates o before changt 16.4 tained. and th 16.5 cosity i relative affect t 17. Inc 17.1 17.1. thermo 2C seller. 17.1. 280 me being r . DUPO 50297691 60 min ilibrating 't of the division n these hoint of ar in a 2 min. and note the bar nt. Read :move the )o not use ttings by > the det baking ;one and adequate atus and iponding D 3451 steady torque transducer deflection. 65-deg angle by means of an exterior lever. 16.2 Apparatus--Weissenberg rheogoniometer21 with at 17.1.3 Tin Plate Panel, 8 by 11 in. (203 by 280 mm). least capability for constant-speed rotational shear, hightemperature electric oven, and cone and plate shearing surfaces. 16.3 Procedure: 16.3.1 By consulting the rheogoniometer instruction manual, select the cone, plate, and torsion wire adequate to measure the largest anticipated viscosity in no more than 10 s. After alignment of the cone and plate, use the electric oven to bring them to the baking temperature of the coating (as agreed upon between the purchaser and the seller), or to a few degrees above that temperature. 16.3.2 As quickly as possible, with the air bearing func tioning, open the oven, raise the cone a few inches, pour sufficient powder to fill the volume between the cone and the 17.1.4 Analytical Balance, sensitive to 1.0 mg. 17.1.5 Steel Pellet Mold Press22 and knockout rod to make pellets 0.25 in. (6 mm) thick by 0.50-in. (12.7-mm) diameter. 17.1.6 Stop Watch. 17.1.7 Steel Rule. 17.2 Procedure: 17.2.1 Weigh out 0.50 g of coating powder and transfer to the steel pellet mold. Press to 0.25-in. (6-mm) thickness and push the pellet out of the mold with the knockout. 17.2.2 Place the pellet on a tin plate panel in a Vh-in. circle scribed or marked on the panel. 17.2.3 Place the panel holding the pellet(s) on the metal plate onto the center of the plate, and lower the cone rack assembly in the oven in a horizontal position. Close the sufficiently to close the oven. Continue to lower the cone oven door quickly. Allow the assembly to remain in the until the proper gap between the cone and plate, as specified horizontal position for 3 min. by the manufacturer of the rheogoniometer, has been 17.2.4 Tilt the rack assembly holding the panel to 65 deg reached. from the horizontal without opening the oven door and 16.3.3 Start the plate rotating at t to 5 rpm, with the allowing the oven to cool. Allow the rack and panel to torque transducer at the largest possible full-scale setting. Caution--Stop the plate rotation should the full-scale torque be exceeded since this may damage the instrument. Start again at a lower rpm. Record torque reading at this rpm. At several lower rotational speeds, record rpm, steady torque reading and the ratio of torque to rpm until the ratio ofthese two becomes essentially constant, indicating a low shear rateNewtonian (constant viscosity) behavior. remain in this position for 30 min. 17.2.5 After 30 min remove the panel from the oven and allow to cool to room temperature. Measure the amount of flow from the original diameter and line scribed on the panel. 17.3 Report--Maximum flow in millimetres from the original diameter. 16.3.4 If lack of sensitivity prevents measurements at low shear rates, repeat the above procedure with a more sensitive torsion wire. If there is no low shear rate Newtonian region N' 8--A control pellet if possible of known reactivity and flow should be run in each test Sample material should be stored in sealed polyethylene bags prior to use and likewise pressed pellets should be evident, the powder may be crosslinking or increasing in stored in a desiccator or sealed bags to prevent moisture absorption. viscosity because of loss of volatiles. Repeated measurements N' 9--The 0.5-g charge should be sufficient for most powders on the same specimen at a given shear rate should indicate this. Several measurements made quickly at very low shear rates on fresh specimens may allow calculation of viscosities with a cured specific gravity of 1.1 to 1.4. For heavier resins, it may be necessary to increase the pellet weight. Ifso, this should be recorded as a variance in specimen size. before crosslinking or volatile loss causes a significant change. 16.4 Report--The viscosity and shear rate values ob tained, the value of the low shear rate Newtonian viscosity and the temperature at which the test was conducted. 18. Density and Specific Gravity 18.1 Apparent Density--Determine iri accordance with Method A of Test Method D 1895. 16.5 Precision--Repeatability and reproducibility of vis 18.2 Bulk Factor--Determine in accordance with Test cosity readings at any given shear rate should be within 10 % . Method D 1895. relative. However, sample age and storage history may. well 18.3 Specific Gravity--Determine in accordance with affect the results obtained. Test Method D 153 or as follows. 18.3.1 In place ofthe pycnometer, a weight-per-galion cup 17. Inclined Plate Flow Test 17.1 Apparatus: 17.1.1 Constant-Temperature fonvection Electric Oven, thermostatically controlled to maintain temperature of 150 2C or as agreed upon between the purchaser and the seller. 17.1.2 Metal Plate Rack Assembly, 8 by 11 in. (203 by 280 mm) that fits into inner oven chamber and is capable of may be substituted. Because of its wide opening, the cup allows ready transfer of powder without loss. In addition the powder can be more readily wet with kerosine (or other suitable carrier agreed upon between the purchaser and the seller) by thorough use of a glass stirrer to remove the entrapped air. Care must be exercised to return any powder particles adhering to the glass rod to the weight per gallon cup to ensure accuracy of the method. being maintained in either a horizontal position .or at a31 31 Weissenberg Rheogoniometer is available from Diano Corp., Midwest Technical Center, 1866 Production Dr, Louisville, KY 40299. " Pair Calorimeter Pellet Press, Cam and Cover type, stainless steel die with standard cavity for making `/2-in. diameter pellets up to V2 in. thickness obtainable from Fisher Scientific Co., Pittsburgh, PA, has been found suitable. An equivalent may be used. 511 DUP050297692 # D 3451 APPLICATION PROPERTIES 19. Determining the Relative Deposition Efficiency of Or ganic Polymeric Powders on Moving Targets 19.1 Summary of Method--The method essentially con sists of spraying powder at a known flow rate on a number of similarly shaped targets moving at a known rate past a powder spraying device mounted in a spray booth. 19.2 Apparatus: 19.2.1 Set of Targets, consisting of 15 flat steel panels 6 by 36 by 0.063 in. (152 by 915 by 1.6 mm) wrapped in aluminum foil, (Use other targets as agreed upon between the purchaser and the seller.) The panels should have holes drilled at one end for hanging from a conveyor. The aluminum foil should be of the lowest possible temper and should be 13Vi by 37 by 0.0015 in. (340 by 940 by 0.04 mm) (these characteristics have been found to be the best for easy wrapping of the panels). Other tempers, thicknesses, and dimensions may be used, however (for example, regular commercial aluminum foil is satisfactory). 19.2.2 Fifteen Target Hangers constructed so that the targets will hang from the conveyor in one plane within Vi in. (13 mm) with the flat surfaces perpendicular to the source of the powder spray. The target hangers should be long enough so the source of the powder spray can be pointed at the center of the targets. 19.2.3 Powder Flowmeter, consisting of a vacuum cleaner attached to a small vacuum chamber (powder receiver) constructed as shown in Fig. 5. 19.2.4 Balance, sensitive to 100 mg. 19.2.5 Balance, sensitive to 1 mg. 19.2.6 Stop Watch, accurate and readable to Vs s. 19.2.7 Powder Spray System. 19.3 Procedure: 19.3.1 Cut the number of aluminum-foil wrappings nec essary for the desired number oftests and number (with a felt tip pen, grease pencil, etc.) on one comer. If the available balance can weigh the entire target, weigh the panels with the aluminum-foil wrappings. If the balance cannot weigh the entire target, weigh the aluminum-foil wrappings alone. Record the numbers and corresponding weights. 19.3.2 Wrap the targets with the foil. The best method of doing this is simply to lay the foil on a flat surface with the numbered side down. Place the target on the foil so that it is centered on the foil and Vz to 1 in. (13 to 25 mm) from the long edge of the foil. For convenience, the top of the target (where the hanger holes are) should be at the numbered end of the foil wrap. Fold the Vz to 1-in. (13 to 25-mm) piece of foil over the edge of the target, creasing it firmly. Then turn the panel over so that it wraps the foil around itself, and crease the new edge firmly. Then him the panel over again (this will fold the remaining foil over) and crease it firmly. 19.3.3 Determine the conveyor speed by measuring the distance between two points on the conveyor track at least 10 ft (3.05 m) apart and by measuring, with the stop watch, the time it takes a location on the conveyor chain to travel the distance between the two points. If possible, adjust the conveyor speed to as close to 10 ft/min as possible (2 %). 19.3.4 If possible, hang the 15 targets on the conveyor on 12 in. (305 mm) centers far enough ahead of the spray booth to allow the conveyor to come up to speed (at least 1 min travel) or for this test, 10 ft (3.05 m). 19.3.5 Break up any powder agglomerates in the powder by mixing or sieving before adding to the powder hopper. Determine the powder flow by first weighing the vacuum cleaner bag with the balance and then installing it in the bag chamber. The vacuum cleaner bag alignment holes should go on the alignment pins on the bag chamber. Install the cover on the bag chamber (simply place on bag chamber). Start the vacuum cleaner and adjust the damper so that very little air is felt moving through the hole in the cover (vacuum in the vacuum bag should be 0.3 to 0.7 in. (8 to 17 mm) of water, vacuum in the flowmeter should be 1.5 to 2.5 in. (38 to 64 mm) of water). 19.3.6 Insert the powder spray device into the opening in the top of the powder flowmeter and turn on the dust collector. Turn on the powder spraying device for 30 or 60 s. (Caution--Be sure high voltage is turned off or, if that is not possible, at the lowest possible adjustment), measuring the time with the stop watch. Disassemble the powder flowmeter and reweigh the vacuum cleaner bag on the balance. The increase in weight divided by the time the powder was flowing is the rate of powder flow. The powder in the vacuum cleaner bag can be recovered simply by tearing the bag in half and dumping the powder in the booth or hopper. 19.3.7 Adjust the powder flow, if possible, to 300 g/min 5 % by successive process changes. Also adjust or record, or both, all the process variables possible including the fol lowing: 19.3.7.1 The powder and its state of use, 19.3.7.2 The particle size distribution if available, 19.3.7.3 The high-voltage power supply output potential and output current, 19.3.7.4 The resistor in the gun, 19.3.7.5 The potential of the powder gun's charging tip, 19.3.7.6 The distance between the target and the charging tip, 19.3.7.7 The pattern adjustment mechanism (measure such things as the relative locations of the parts), 19.3.7.8 The conveyor speed, 19.3.7.9 The powder flow, 19.3.7.10 The powder collector system air flow or some pressure which changes as a function of air flow only, 19.3.7.11 The powder transfer air flow and air pressure, 19.3.7.12 The powder quantity control pressure or what ever variable controls this, 19.3.7.13 For fluidized beds; air flow, air pressure, the amount of powder, and bed depth, 19.3.7.14 Other variables such as vortex air, dosing air, powder density air, pattern air, etc,.and 19.3.7.15 The atmospheric variables: temperature, baro metric pressure, and humidity. 19.3.8 Mount and level the powder spray device in the spray booth so that it is aimed at the centers of the targets as they pass. Position it so that its charging tip is 8 Vz in. (203 13 mm) from the plane in which the targets will pass. 19.3.9 Turn on the powder flow, adjust the high voltage to 60 1 kV (use other voltages as agreed upon between the purchaser and the seller), turn On the powder collection system, etc. Start the conveyor and spray the targets after all other systems seem to be operating normally and powder is spraying into the spray booth. 19.3.10 Afh remove the U powder off of' the targets in; mended for th js also an exc retained after preweighed 5place this in C 19.3.11 Aft and pull the a as soon as pos This facilitatf because the cc and become-' handle. If nec oven. After tfc foil wrapping: 19.3.12 W. pings from tb each end of because they relative to t powder adde powder and powder was r wiped off to 19.3.13 G Calculate tb lowing equat %E where: % E = pe; Wrr p = m< Vc = Co -- dis QP - po % R = pe (1 19.3.14 ` coating, ca following e. where: V_ = coe Wp = wei n = nu: WB = me 19.3.14.1 indicates tl This is due tion, some sometimes powder clo 19.3.15 results agn 512 DUPO 502 97693 owder opper, icuum he bag uldgo cover art the -tie air in the water, to 64 mg m i dust r 60 s. is not ig the meter The r was n the ng the apper. min ird, or e fol- :ential ; tip, arging ;asure ;ome ire, diat- the air, baro- n the ;ets as .(203 SS. age to :n the sction ter all der is > D 3451 19.3.10 After spraying the targets, stop the conveyor and remove the targets, taking care not to knock or jar the powder off of them. If it is desired to cure the powder, place the targets in an oven for the time and temperature recom mended for the specific powder being used. If necessary, this is also an excellent time to determine the weight percent tetained after curing the powder. Weigh 1 g of powder in a preweighed 5-in. (127-mm) diameter aluminum foil "pan." place this in the oven along with the targets. 19.3.11 After curing, remove the targets from the oven and pull the aluminum foil down 1 to 2 ft (305 to 610 mm) as soon as possible using asbestos or thick workman's gloves, this facilitates the final removal of the aluminum foil because the coated foil tends to contract slightly with cooling and become very difficult to remove when cool enough to handle. If necessary, also remove the pan of powder from the oven. After they are reasonably cool, remove the aluminumfoil wrappings, if they are to be weighed alone. 19.3.12 Weigh the center 11 targets or aluminum wrap pings from the center 11 targets excluding the two targets on each end of the target set (The end targets are excluded because they tend to collect excessive amounts of powder relative to the other targets.) Determine the amount of powder added to each target. If necessary, weigh the pan of powder and determine the weight percent retained. If the powder was not cured, the targets may be blown off and then wiped off to prepare them for the next test. 19.3.13 Calculate the mean weight of powder deposited. Calculate the percent deposition efficiency using the fol lowing equation: % E = (Wp x Vc x 10 000)/U)T xQpx% R) where: % E -- percent deposition efficiency, Wp = mean powder deposition, g, Vc = conveyor speed cm/min, Dt = distance between target centers, cm, Qp = powder flow, g/min, and % R -- percent by weight powder retained after curing (100 % if not cured). 19.3.14 To determine the variation in application of the coating, calculate the coefficient of variation using the following equation: 2 Wf - nWA1'2 n- 1 / WP where: F = coefficient of variation %, Wp - weight of powder on a foil wrapping, g, _ = number of targets used (11), and Wp = mean powder deposition, g. 19.3.14.1 If the coefficient of variation exceeds 10% it indicates that the powder cloud is fluctuating excessively. This is due usually to poor (slugging) powder pump opera tion, sometimes to unstable booth air flow profiles, and sometimes to unstable air flow patterns created by spray gun powder cloud control system. 19.3.15 Repeat the above procedure until two consecutive j results agree within 10 %. Use the set of conditions under which these results were obtained as a standard to which to relate future work. It is wise to run the test within the standard conditions at the beginning and end of each day. If results do not agree within 10 % the day's work should be suspect. Results will vary from day to day and even during the day due to variables beyond the user's control. Long term variations can even be as large as 50 %. Tests run with different powders or under different conditions should have the results reported in terms of the standard test results. For example, if die efficiency results under the standard condi tions were 50 % with one powder and 75 % with another powder, the second powder would be 50 % more efficient than the first powder. 19.4 Report: 19.4.1 Report the variables and their values as recorded for 19.3.7. Report the percent deposition efficiency and its coefficient of variation, the percent efficiency compared to the average percent efficiency obtained using the standard conditions on the day of the test. 19.5 Precision--Deposition efficiency results should be repeatable within 10 % during a day. PHYSICAL PROPERTIES OF POWDER COATING 20. Panel Preparation 20.1 Treatment of the Substrate--Clean and prepare test panels in accordance with one of the following standard test methods or recommended practices or as agreed upon between the purchaser and the seller: 20.1.1 Method D 609. 20.1.2 Practices D 1730. 20.1.3 Practices D 1731. 20.1.4 Practices D 1732. 20.1.5 Method D 1733. 20.1.6 Practices D 2092. 20.1.7 Test Method D 2201. 20.2 Priming and Sealing--In many instances, the use of a primer, primer surfacer or sealer is required. The type, application, and treatment of any undercoat system should be agreed upon between the purchaser and the seller. 20.3 Application of Powder Coatings--The coatings may be applied by fluidized bed, electrostatic spray, or other methods. 20.4 Curing ofPowder Coatings: 20.4.1 Fuse or bake the powder coating to a uniform film according to the established schedule and temperature and age as agreed upon between the purchaser and the seller before running tests. 20.4.2 The powder coating should be overbaked to deter mine the time/temperature effect on the physical and chem ical properties in accordance with Recommended Practice D 2454. 20.5 Measurement ofFilm Thickness--Since the proper ties of a powder coating can vary considerably with its thickness, it is important to know the film thickness. Measure the film thickness in accordance with Test Method D 1005, D 1186, or D 1400. 21. Abrasion Resistance 21.1 Determine the abrasion resistance in accordance with Test Method D 658, D 968, or D 1044. 513 DUP050297694 3451 22. Adhesion 22.1 The powder coatings of a specified thickness and over a specified substrate as agreed upon between the purchaser and the seller is subjected to an adhesion test to determine the degree of attachment the coating has to the substrate. 22.2 Determine the adhesion of the powder coating to the specified substrate in accordance with Test Methods D 2197 or D 3359. 23. Chemical Resistance 23.1 Coating systems frequently come into contact with various chemicals which may have an effect on the proper ties of the system. Failure, when it occurs, is usually in the form of discoloration, change in gloss, blistering, softening, swelling, or loss of adhesion. 23.2 Household Chemical Resistance--Determine the ef fect of chemicals in accordance with Test Method D 1308. 23.3 Detergent Resistance--Determine the resistance to failure when immersed in a detergent solution in accordance with Practice D 2248. 24. Chip Resistance 24.1 In many end uses, the ability of a powder coating to withstand sudden impact from stones, gravel, etc., without being loosened from the substrate is important. 24.2 Determine chip resistance in accordance with Test Method D 3170. 25. Color--Pigmented Coatings 25.1 The colors of opaque objects such as coated surfaces may be specified by visual or instrumental requirements. 25.2 For visual evaluation, determine the color of a coated surface in accordance with Method D 1535. 25.3 Determine the color of a coated surface instrumentally in accordance with Method E 308. 26. Color Difference--Pigmented Coatings 26.1 The color difference between two homogeneously colored opaque films may be determined by visual evalua tion or by instrumental means. 26.2 Determine color differences visually in accordance with Practice D 1729 or instrumentally by Method D 2244. 27. Cracking Resistance 27.1 The cracking resistance test is designed to give an indication of the resistance of a coating system to cracking and checking caused by temperature and humidity changes. Some factors which may affect results are type of substrate, substrate thickness, undercoat, topcoat, and film thickness. 27.2 Determine cracking resistance in accordance with Test Method D 2246. 28. Elongation 28.1 An elongation test may give an indication of the flexibility of a powder coating. It can also show whether there is any change in flexibility due to the aging of the film. 28.2 Determine elongation in accordance with Test Method D 522 or D 1737. 29. Filiform Corrosion Resistance Salt Spray 29.1 Filiform corrosion is a type of corrosion that ( ( r under coatings on metal substrates and is characterized by a definite thread-like structure and directional growth. 29.2 Determine the susceptibility of a powder coating on a metal substrate to this type of corrosion by Test Method D 2803. Q 30. Gloss 30.1 Determine the gloss of a powder coating in accord, ance with Test Method D 523. 31. Hardness 35.1 Salt sp determining tl coaditions of h Jue accelerated jture, pH, co: physical parair jLibstrate, the gating is scri yithin the cab panels and the upon between 35.2 Test f< ytethod B 117 31.1 Determine the hardness of powder coating in accordance with Test Method D 1474 using either Method (Rnoop Indentation Hardness) or Method B (Pfund Indentation Hardness). 31.2 Other methods of determining hardness are widely used in some industries and may be used as agreed upon between the purchaser and the seller. 32. Impact Resistance 32.1 Films formed from powder coatings may be subject to sudden impact in certain end uses. Determine impact resistance in accordance with Test Method D 2794. 33. Outdoor Exposures 36. Water Re 36.1 Testin determining t. [jigh humidity usually evider adhesion whic tion of the ab 36.2 Deter; of high humic 36.3 Deter of water imm test is best sx soaked in wai 33.1 While the accelerated tests given elsewhere in this recommended practice are intended to enable prediction of probable performance, actual outdoor exposures should be made on coatings intended for exterior use. Usage of paint systems is so varied that no one set of conditions (length or place of exposure) can be given in this practice to cover all situations. These conditions as well as the type of substrate, substrate preparation, etc., should be agreed upon between the purchaser and the seller. However, it is suggested that unless otherwise agreed upon, panels for outdoor exposure should be prepared in accordance with Section 19 of this practice. 33.2 Many properties of powder coating films should be evaluated periodically throughout the outdoor exposure period. These properties may be evaluated as follows: 33.2.1 Blistering--Test Method D 714. 33.2.2 Chalking--Test Method D 659. 33.2.3 Checking--Method D 660. 33.2.4 Cracking--Test Method D 661. 33.2.5 Rusting--Method D 610. 33.2.6 Erosion--Test Method D 662. 33.2.7 Flaking--Test Method D 772. 34. Print Resistance 37. Safety ar 37.1 This aging, shippi: and applicati decorative cc volumes of p 37.2 Whe; ical aspects ; Administrati 37.3 Pack 37.3.1 Ci containers plastic-linec 37.3.2 D fied as to t manufactur 37.4 Shi, 37.4.1 Pc manner to t 37.4.2 Bi died in a m Precautions of the powd 37.5 Slot 34.1 A print test may be used to determine the degree of themoplasticity or solvent retention of a film and hence whether the product can be safely stacked or packaged and, in the case of a thermoplastic film, at what temperature the film prints or mais. The print test can also determine the degree of marring due to pressure. 34.2 Determine the imprinting and thermopiasticity of a powder coating film in accordance with Test Method D 2091. 514 JL DUP050297695 D 3451 hat occurs -`rized by a th. roating OJ1 st Method n accord. n accordlethod id Inden'e widely ed upon 2 subject * impact in this ction of ould be of paint ngth or over all bstrate, >etween ed that tposure of this aid be losure ;ree of hence i and, re the \e the y of a ethod 35. Salt Spray Resistance 37.5.1 All containers must be sealed when not in use. 3J.I Salt spray testing of coatings may be helpful in j tennining their resistance to failure in service under Editions of high humidity and salt concentrations. Under accelerated conditions of the laboratory test the temper- 1 ture, pH, concentration of the salt solution and other | al,ysical parameters can be controlled. The selection of the j Pjbstrate, the coating system, the manner in which the I gating is scribed, the location or position of the panels i Ljthin the cabinet, the length of the test, the inspection of .nels and the method of reporting results must be agreed f^oii between the purchaser and the seller. I 37.5.2 Temperature and relative humidity during storage should not exceed 80F (27C) and 50 %, respectively, or as specified on the label. 37.6 Precautions in Handling and Application: 37.6.1 All metal equipment must be properly grounded. 37.6.2 The fluid bed must be cleaned periodically to ensure proper operation. 37.6.3 Under certain conditions organic powders may be subject to dust explosions. Trade association bulletins such as the National Fire Protection Association Bulletins No. 33, Spray Finishing and No. 654, Dust Explosion Prevention-- *35.2 Test for salt spray resistance in accordance with I PLastics Industry, may be helpful in identifying conditions Method B 117. | and minimizing their occurrences. 37.6.4 Spraying: Water Resistance 37.6.4.1 Spray booths, dust collectors, and ducts should be built with smooth surfaces to facilitate cleaning. If 36.1 Testing of coating systems with watef is helpful in ! possible, surfaces should be of a material to which the (jetermining their resistance to failure under conditions of powder will not stick. (jjgh humidity or water immersion. Failure in water tests is 37.6.4.2 During nonoperating periods all equipment usually evidenced by blistering, dulling, softening, or loss of I should be flushed with air or the manufacturer's recom- adhesion which does not disappear or recover upon evapora i mended procedure should be followed. tion of the absorbed water. 37.6.5 Blending--If reclaimed or recycled powder is to be 36.2 Determine the resistance to failure under conditions ; blended with virgin material, a suitable device for sifting, 0f high humidity in accordance with Practice D 1735. | drying, and blending should be used. 36.3 Determine the resistance to failure under conditions i 37.6.6 Dust Collection and Ventilation--All handling and of water immersion in accordance with Practice D 870. This [ application equipment should be fitted with a suitable dust test is best suited for coating systems that will actually be collector and filter system. soaked in water during service. 37.6.7 Suitable electrical grounding is required. Precau- ; tions are necessary to ensure ratio of powder to air are held 37. Safety and Handling Precautions 37.1 This recommended practice covers the safe pack aging, shipping, receiving, storage, and handling during use and application of organic powders used for protective and decorative coatings. Procedures for handling large and small volumes of powder are included. 37.2 Where required, attention shall be directed to ecolog ical aspects and pertinent Occupational Safety and Health Administration (OSHA) regulations. 37.3 Packaging: 37.3.1 Container--For small and medium operations, ; below or above the explosive mixture. : 37.7 Ecology: 37.7.1 Exhaust stacks should be equipped with dust col; lectors or absorbers or both to avoid air pollution. 37.7.2 Waste Disposal--Powder must be disposed of in I the manner governed by local laws and regulations. 37.8 OSHA Requirements: \ 37.8.1 Operator Safety--All personnel should be equipped with suitable air masks, gloves, and any other specified devices for personal protection. 38. Data Report containers designed to give moisture protection, such as 38.1 The report shall include the following: plastic-lined boxes or drums, should be used. 38.1.1 Complete identification of the powder coating 37.3.2 Labeling--All containers should be clearly identi material tested, fied as to type material, color, batch number, and date of ' i 38.1.2 Description of specimens, including numbers, manufacture. preparation method, and thickness of coating, 37.4 Shipping and Receiving: | 38.1.3 Temperature of test if other than specified by test 37.4.1 Palletizing--Containers should be palletized in a method, manner to avoid crushing or packing. 38.1.4 Type and manufacture of test equipment, 37.4.2 Bulk Shipment--Large shipments should be han 38.1.5 All specific information called for on the individual dled in a manner agreeable to the purchaser and the seller. test method report, Precautions should be taken to avoid hard packing or caking | 38.1.6 Test results as calculated or observed values on the of the powder. basis of data, median or mean value, and 37.5 Storage: 38.1.7 Date of test. , The American Society for Testing and Materials takes no position respecting the validity ofany patentrights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk ot infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are invited either for revision ot this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will, receive careful consideration at a meeting ot the responsible technical committee, which you may attend. If you feel that your comments have not received a talr hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. Ai 515 DUP050297696 4 jjjro Designation: D 3456 - 86 (Reapproved 1991)ei Standard Practice for Determining by Exterior Exposure Tests the Susceptibility of Paint Films to Microbiological Attack1 This standard is issued under the fixed designation D 3456; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the. year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {<) indicates an editorial change since the last revision or reapproval. '1 N' --Keywords were added editorially in July 1991. 1. Scope 1.1 This practice provides guidelines for determining the susceptibility of paint films to microbiological attack: on exterior exposure. While it is recognized that various organ isms may occur on an exposed coating, the specific types of organisms are mainly of academic interest. The degree to which microbiological discoloration occurs is the primary concern. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 1006 Practice for Conducting Exterior Exposure Tests of Paints on Wood2 D1849 Test Method for Package Stability of Paint2 D3274 Test Method of Evaluating Degree of Surface Disfigurement of Paint Films by Microbial (Fungal or Algal) Growth or Soil and Dirt Accumulation2 3. Summary of Practice 3.1 Simple observation of a coated object subjected to exterior exposure is considered a practical and reliable method for determining the degree that microorganisms discolor the coating. However, this applies to a specific coated object exposed under a given set of conditions. It should be recognized that there are critical factors that influence the amount of fungal growth that may occur on the same coated object when exposed to other conditions. These factors include the geographic location, local atmospheric conditions such as the dust and pollen content of the air, angle of exposure, degree to which the coating is subjected to weathering, effects of moisture and sunlight, the substrates on which the coating is applied, and the coatings in the paint system under test. The latter factor includes the stability of the coating while packaged in the container, as well as the composition of the coatings included in the total system and 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint, and Related Coatings and Materials and is the direct responsibility of Subcommittee DOt.28 on Biodeterioration. Current edition approved March 27, 1986. Published May 1986. Originally published as D 3456 - 75. Last previous edition D 3456 - 75 (1981)*' 2 Annual Book ofASTM Standards, Vol 06.01. the thickness of each coating applied. Thus, while microorganisms occur on the surface of the last film applied, the degree of microbiological growth that will occur is also influenced by the composition of the undercoats. All the above factors should be considered in the selection of a coating resistant to discoloration by microorganisms. 4. Significance and Use 4.1 The growth of fungi and algae in and on the surface of paint films represents a major cause of discoloration or disfigurement of painted surfaces. This practice covers the preparation of coatings for testing, their application on substrates, and the arrangement of the coated panels on exterior test fences to determine the degree of microbiolog ical attack that may occur on the surface of the coatings over a period of time. This practice is intended to provide guidelines for, and a discussion of, the various factors critical in selection of exterior coatings resistant to discoloration ( 9 disfigurement by algae and fungi. 5. Preparation and Application of Coatings 5.1 Conditioning of Coatings Prior to Application--Indi vidual coatings to be used in the paint system should be properly aged under suitable conditions prior to testing. Hydrolysis, amalgamation, absorption, and other physical and chemical changes that may have a profound influence on the resistance of a coating to microorganisms usually increase with increasing temperature. It is recognized that actual storage periods of paints prior to use may vary from one to several years, and the peak temperature encountered may be as warm as 160F (70C). However, a recommended conditioning period consists of 1 year at room temperatures or 1 month at 125F (50C) as in Test Method D 1849. The conditioning of coatings prior to testing shall be agreeable to the producer and the user in the case of a referee test 5.2 Preparation of Coatings for Application--Prior to application ofthe various coatings to be included in the total paint system, thoroughly reconstitute each coating by appro priate mixing or shaking. At the time of application, there must be no settling, incompatibility, or other stability problem observable in the coating in the container. 5.3 Application of Paint System--Apply each coating ffi the total paint system in an appropriate manner to provide a specified and reasonably uniform film thickness. The pres ence and thickness of different coatings, in the complete system can have a pronounced effect on the degree of microbiological discoloration that will occur. Thus, each paint in the s ipanufacturei agree on the coating in the and the curi: should also 1 paint is 2 day longer than trial and in different pra and the user 5.4. On ei (310 cm2) ir used, expose substrate is t panels of eac referee test, test area be Common pi 36-in. (152 and to use for exposur- ings. 6. Substraf 6.1 Gem paint systei degree of Coated wc algae than perhaps di retention o metal sub influence c inactivate microbiolc that metal because of metal. M growth be characteri by hydrol been usee testing cc ganisms ' In referee ! agreeable | should b designed, are gener; of substi following reasons. 6.2 W is consid may be dimensic | applied ( cracks. I 5 UCtS SUp' ; the nut 516 DU PO50297697 icroor2d, the is also ^11 the 3 of a ace of on or rs the n on ;ls on iologsovef ovide ritical on or Indid be ting, sical nee Uly hat 3m ed led res The eto to otal jrolere lity ; in le a esete of ich D3456 03int in the system must be applied as recommended by the Manufacturer. It is important that the procedure and the user gree on the type of coatings and the spreading rate of each gating in the final test film. The drying time between coats ,,,id the curing time of the total system prior to exposure should also be specified. Recommended practice for house paint is 2 days between coats and no less than 7 days and not j0nger than 1 month prior to the exterior exposure. Induspial and industrial maintenance coatings may require a different practice that should be acceptable to the producer jijd the user. 5.4. On each substrate use a test area not less than 48 in.2 (310 cm2) in size. When only one type of substrate is being uSed, expose at least duplicate panels. When more than one substrate is employed for each exposure condition, duplicate panels of each substrate are not usually required. In case of a isferee test, it is recommended that replication and size of test area be agreed on between the producer and the user. Common practice in the industry is to use 6 in. (nominal) by 36-in. (152 by 915-mm) panels for house paint exposures and to use 12-in. (305-mm) metal panels of various widths for exposures of industrial and industrial maintenance coat ings. 6. Substrates for Testing 6.1 General Considerations--The substrate on which a paint system is exposed can have a significant effect on the degree of microbiological discoloration that may occur. Coated wood surfaces generally support more mold and algae than do coatings on metals or masonry surfaces. This is perhaps due to some nutrients and greater porosity for retention of available moisture in wood surfaces. The type of metal substrate can have either an adverse or beneficial influence on the growth of fungi and algae. Some metals can inactivate certain microbiocides, thereby allowing greater microbiological discoloration. It should also be recognized that metals may also reduce the growth of microorganisms because oftoxic compounds resulting from weathering ofthe metal. Masonry surfaces generally inhibit microbiological growth because of their alkaline nature. However, this same characteristic can contribute to microbiological discoloration by hydrolyzing alkali-sensitive microbiocides that may have been used in the coating. The recommended substrates for testing coatings for resistance to discoloration by microor ganisms vary according to the intended use of the coatings. In referee cases, the substrate for testing shall be mutually agreeable to the producer and the user. Industrial coatings should be evaluated on the surface for which they are designed. Trade sales and industrial maintenance coatings are general-purpose coatings and should perform on a variety of substrates. For such coatings, test exposures on the following substrates are recommended for the indicated reasons. 6.2 Wood Substrates--Sapwood of pine and fir generally is considered conducive to growth of microorganisms. This may be due to nutrients in the wood and to the low dimensional stability, resulting in microcracking of coatings applied on the wood with subsequent mold growth in these cracks. Plywood, hardboard, and other wood-derived prod ucts support varying degrees of fungal growth depending on the nutrient value, degree of moisture absorption, and dimensional stability of the base material. Redwood tends to have better dimensional stability and otherwise has insignif icant effect on the microbiological growth on coatings applied over it. Cedar lumber generally contains compounds that aid in resisting microbiological growth. Both cedar and redwood contain colored extractives that can bleed through coatings to discolor the surface. Some ofthese extractives can also be nutrients that contribute to microbiological growth, resulting in added discoloration. 6.3 Metal Substrates--Iron, galvanized steel, and alu minum are common substrates for paints. Iron and compounds generally inhibit microbiological growth. On the other hand, these metals may react with certain microbiocides to reduce the microbiological inhibition. Cer tain microbiocides can also cause discolored corrosion prod ucts or loss of adhesion by the coating on these surfaces. Aluminum is rather chemically inert and does not itself promote microbiological growth. It may, however, cause loss of microbiological resistance of coatings containing certain mercury compounds because of the amalgamation reaction by aluminum and mercury. This can result in loss of adhesion. 6.4 Masonry Substrates--The extremes of masonry sur faces generally consist of two conditions: fresh surfaces, which are relatively alkaline and free of fungi and algae, and weathered surfaces that are less alkaline and may be discol ored because ofmicrobiological growth. Weathered masonry surfaces represent useful test surfaces since microbiological contamination can grow through inadequately preserved coatings from the underside. Weathered masonry surfaces also offer a relatively uniform surface from panel to panel. Such uniformity is useful in statistically determining the relative effectiveness of various coatings or of various wash solutions for cleaning or "sterilizing" a surface before re painting. Exposures of coatings on both clean masonry panels and weathered panels can provide useful results and both are recommended as test substrates. 6.5 Moldy "Mildewed" Repaint Surfaces--Weathered paint films that are discolored by microbiological growth are also useful in determining the efficacy of wash solutions to clean or "sterilize" an old paint film prior to repainting. Such moldy repaint surfaces also are useful in determining the resistance of a coating system to discoloration due to microorganisms growing through the paint system from the underside. 7. Arrangement of Coated Panels on Exterior Test Fences 7.1 Paint systems should offer long-term resistance to microbiological growth both in completely exposed areas and in shady, protected areas. Where sunlight and moisture are in abundance, chalking will occur. However, chalking is slow to occur in shady areas. Thus, an effective microbiocide for a coating must have long-term light stability, heat resistance, and be sufficiently soluble and toxic to cause microbiological inhibition, and it must have limited solu bility or teachability from the coating system such that it remains in the system for sufficiently long periods of time. Ideally, it should not induce chalking for cleaning of the surface, since such chalking will cause fading or tinted paints. 7.2 The most realistic conditions of exposure can best be realized on the exterior of houses. Unfortunately, buildings 517 DUP0502 97698 # D 3456 with the various substrates and located in desirable localities and geographic locations are seldom available. However, comparisons of various coating systems can be made by exposing coated panels on exterior test fences. Positions of exposure should vary to include completely exposed weath ering conditions and also protection from weathering. The exposed conditions are useful in determining the influence of temperature, sunlight, moisture, various substrates, and subsequent chalking on a coating. The protected, shady exposures are useful in determining the relative microbiolog ical inhibition of coatings in the absence of chalking. 7.3 Construction of test fences for protected or shady conditions can be similar to that given in Practice D 1006 but modified to provide for a larger test area in the protection of an eave. A protected area under an eave facing north best represents the desired conditions. This eave should have a minimum of 18 in. (455 mm) overhang. The panels should be exposed in a lapped position as would be encountered with wood siding on a house. The test area for each system should begin immediately under the eave and continue down the test fence to a point at least 2 ft (610 mm) below an imaginary horizontal line, which is derived by projecting at a 45 angle from the outer edge of the eave, downward and inward to the test panels. Thus, an 18-in. eave would require a minimum of 3.5 ft (1.06 m) of test panels, beginning immediately under the eave down to the bottom edge of the exposure area. The inverted horizontal surface of the soffit under the northerly eave is an ideal test environment as well. Also, this area does not usually collect excessive dirt. Thus, any microbiological discoloration is readily apparent. 7.4 Construction of test fences for exposed conditions can be similar to that in Practice D 1006 but modified to provide for offset panels held at an angle of 5(5) off vertical facing south. Construction should allow exposures such that mois ture falling on the test area of one panel will not drip on the next panels below. 8. Geographic Location of Test Fences 8.1 The climatic and environmental conditions of the test fences should be similar to those of the areas in which the paint system is intended for use. For coatings to be used nationally, it is desirable to expose in warm and humid environments. Exposures should be made in both shady conditions and in direct sunlight. It should be recognized that the microflora occurring in different parts of a country will vary so that mold and algae encountered in one test location may not necessarily be those of another. 9. Periods of Exposure 9.1 The time of the year when the initial exposure is first made can be critical. Because of differences in weather from year to year, results of exposures from one year to another may also vary. In order to compare the tendency for two or more paint systems to become discolored through microbio logical growth, it is advisable that the paint systems be exposed at the same time. It is frequently desirable to include both a positive and a negative control. The negative (fail) control is a paint system known to discolor quite severely under standard exposure conditions and may be used on each panel. A positive (pass) control is a paint system that will perform reasonably well in the same known exposure conditions. 10. Ratings for Microbiological Discoloration 10.1 Ratings should be made in accordance with Test Method D 3274. 10.2 It is desirable to obtain mold ratings prior to initia tion of chalking and erosion, since it is prior to this occurrence that a paint film is most prone to discoloration by spore-cluster type (dirt-like) mold growth. Chalking can occur within several months, or it may never occur, de pending on the paint formulation and its exposure to weathering conditions. Therefore, mold ratings are suggested after 3, 6, 9, 12, 18, and 24 months and yearly thereafter. Make yearly inspections immediately following seasonal growing conditions. Most extensive microbiological growth usually develops during periods of warm and humid weather. Thus, make any ratings of microbiological discoloration immediately following the warm, humid period of the year. 11. Keywords 11.1 exterior, exposure, microbiological paint films The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invitedeither for revision ofthis standard or for additionsI standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments hove not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Pace St., Philadelphia, PA 19103. Ai V kk 1. Scope 1.1 T1 designed substrate at an ele 1.2 t : or produ in atmos 1.3 T applied 1.4 T ations, address the resp appropr. applical 2. Refei ' pT y r V ' r D71< Pai D10( Th D25' D26` Dr E 14 Vt ,, k . w . k 3. Sigi 3.1 ; expanc change. | splits, t ; in surf; where ; continr not po 'This and Rela mittee D CuiTei publishec 2 Ann: 3 Ann. 518 i DUP0502 97699 used imid hady lized mtry ` test a Designation: D 34S9 - 87 Standard Test Method for Humid-Dry Cycling for Coatings on Wood and Wood Products1 first from Jther 'o or 3bios be :lude (fail) erely i on that >sure Test litiathis nby can dee to :sted ifter. onal )\vth ther. ttion ear. This standard is issued under the fixed designation D 3459; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covens the evaluation of coatings designed for use on interior wood and wood products substrates by exposure alternately to low and high humidity 3t aa elevated temperature. j.2 This test method is applicable to any coated material of product that is affected either entirely or partly by changes U atmospheric relative humidity. 1.3 This test method applies only to those coatings applied in sufficient quantity to form a continuous film. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D333 Test Methods for Clear and Pigmented Lacquers2 D714 Test Method for Evaluating Degree of Blistering of Paints2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D2571 Guide for Testing Wood Furniture Lacquers2 D2691 Test Methods for Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products2 E 145 Specification for Gravity-Convection and Forced- Ventilation Ovens3 3. Significance and Use 3.1 Wood substrates and the coatings applied to them expand and contract to different degrees as the humidity changes, causing stresses that may produce checks, cracks, splits, blisters, swelling, loss of adhesion, and various changes in surface appearance. This test method is intended for use where the coating is applied in sufficient quantity to form a continuous film on the wood or wood product substrate. It is not possible to make any direct correlation between the 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint d Related Coatings and Materials and is the direct responsibility of Subcom| aittee D 01.55 on Factory-Applied Coatings on Preformed Products. Current edition approved May 29, 1987. Published July 1987. Originally Published as D 3459 - 75. Last previous edition D 3439 - 73 (1981)". j 2 Annual Book ofASTM Standards, Vol 06.01. i 3 Annual Book ofASTM Standards, Vol 14.02. ! i, results obtained from humid/dry cycling and the results expected in a specific period of time in service because of variations resulting from geographic locations, location within the building, care of the panel (such as waxing), and variations within materials involved. 4. Test Panels and Panel Preparation 4.1 Test panels shall be regular production finished panels if available. 4.2 If regular production finished panels are not available the purchaser and the seller shall agree upon the following variables: type of wood or wood substrate, sanding method(s) and paper(s), sealer(s) or toner(s), fillers), stain, primer or basecoat, print(s), and topcoat(s), methods of application, and the number of surfaces to be coated. If rotary-cut veneered panels are used, it should also be agreed whether the veneer is to be open or close faced. 5. Apparatus 5.1 Oven--a gravity-convection or forced-ventilation electrically heated oven meeting the requirements of Specifi cation E 145 and providing a continuous temperature of 122 3.5F (50 2C). 5.2 Constant Elevated-Temperature and ConstantHumidity Chamber, maintained at a relative humidity of 97 2% and a temperature of 122 3.5F (50 2C). 5.3 Constant-Temperature and Constant-Humidity Cham ber, maintained at a relative humidity of 50 5 % and a temperature of 73.5 3.5F (23 2C). 6. Test Specimens 6.1 Test specimens shall be large enough to be representa tive of the material or product and to permit easy observa tion of possible defects. This usually means a minimum area of approximately 12 by 12 in. (300 by 300 mm). 6.2 Unexposed control specimens of each coating or coating system or product tested shall be held in reserve in a constant-temperature and constant-humidity area (5.3) to prevent any changes. 6.3 Whenever possible, comparative control specimens of a similar material or product with known service character istics should also be exposed. 6.4 Three specimens are usually adequate unless a lack of uniformity is suspected in the substrate, coating, or coating system. 7. Conditioning 7.1 Place the specimens in a conditioned room or chamber (5.3) so that air is free to circulate on all sides of DUPO 502 97700 D 3459 each specimen so as to avoid localized overheating. Allow them to remain there 14 days. 8. Procedure 8.1 Measure the dry film thickness of the coating system on the control panel to the nearest 0.1 mil (2.5 pm) by an appropriate method such as Test Methods D 1005, Methods D2691, or an Optical Surfacer Analyzer.4 The results of humid dry cycling are directly affected by the dry film thickness as well as by the coating system itself. 8.2 After conditioning measure thickness of each spec imen to the nearest mil (25 pm) at a marked location about 1 in. (25 mm) from one edge and midway along one side at the beginning and after each change of conditions. 8.3 Place the specimens in the oven maintained at 120 3.5F (50 2C) (5.1) so that air is free to circulate on'all sides of each specimen to prevent localized overheating. After 48 h remove the specimens from the oven and place them in the high-humidity elevated-temperature chamber (5.2) so that air is free to circulate on all sides of each specimen. Leave the specimens in the humidity cabinet 48 h. The period of 48 h of dry heat followed by 48 h of humid heat constitutes one cycle. Expose the specimens to the number of cycles as agreed upon between the purchaser and the seller. 8.4 At each change of conditions during cycling, visually inspect each specimen under a strong light and at various 4 Gardner, H. A. and Sward G. G., Paint Testing Manual, 13th edition, ASTM STP 500, ASTM, 1972, angles to the light for possible damage or change. Note any change in or damage to each specimen. Damage may be found in the base material (plywood, hardboard, flakeboard solid wood, etc.) or in the coating, in a finish or overlay on the substrate material. Some defects that may occur as a result of humid/dry cycling are as follows: checks, cracks, splits, blisters, (see Test Method D 714) raised grain, local ized lumps or swelling, photographing of substrate through the coating, loss of particle adhesion, loss of adhesion in glue lines, change in the dimensions of the overlay, changes in surface color, gloss, or hardness, cohesion loss in the coating. If open-faced rotary-cut veneer has been used, checking may result from this fact. 9. Report 9.1 Report the following information: 9.1.1 Complete description of the test material and the comparative control material, 9.1.2 Size and number of the specimens, 9.1.3 Dry film thickness of the material under test and the control (comparison material). 9.1.4 Number of cycles agreed upon between the pur chaser and the seller, 9.1.5 Any deviations from the standard procedure, and 9.1.6 Defects or changes as described under 8.4. 10. Precision 10.1 Since the observed changes can take several forms no numerical values have been developed, and meaningful estimates of precision cannot be given. Round-robin tests showed that cooperators can obtain satisfactory agreement in ranking of results. The American Society for Testing and Materials takes noposition respecting the validity of any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard ere expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited eithertor revision ofthis standardor for additionalstandards and should be addressed io ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. D i. Scope 1.1 Tt of evapo Shell Th: applied i varnish, carbons 1.2 T rate ustr Method A Method B- 1.3 1 the volt the dis[ syringe. 1.4 : ations, addresi the res approp applies hazard 2. Re! 2.1 D8 t! E1 3. Su 3.1 of flit' `Th Paint Subcor rials. Cur publish 2T1 York: Subcoi Paint' Techn *A DUP05 029 7701 . Note any ?e may be lakeboarc^ overlay occur as $ ks, cracks, rain, local' te through ion in glUe ihanges in le coating, eking may Designation: D 3539 87 Standard Test Methods for Evaporation Rates of Volatile Liquids by Shell Thin-Film Evaporometer1 2 3 This standard is issued under the fixed designation D 3339; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. These test methods have been approved for use by agencies of the Department of Defense andfor listing in the DoD Index of Specifications and Standards. il and the :st and the the pur- ire, and . forms no teaningfu] obin tests eement in |. Scope [.1 These test methods cover the determination ofthe rate flf evaporation of volatile liquids of low viscosity using the Shell Thin-Film Evaporometer, The test methods have been applied to a wide range of volatile liquids, including paint, varnish, and lacquer solvents and thinners to various hydro carbons and to insecticide spray-base oils. 1.2 The test methods for the determination ofevaporation ,ate using the thin-film evaporometer are: Sections Method A2,3--Manual Recording................................................. Method B--Automatic Recording................................................ 5 to 11 12 to 17 1.3 The test methods are limited only by the viscosity of the volatile liquid which must be sufficiently low to permit the dispensing of an accurately measured specimen from a syringe. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Notes 1 and 2. 2. Referenced Documents 2.1 ASTM Standards: D89-1 Test Methods for Specific Gravity of Liquid Indus trial Chemicals4 E 1 Specification for ASTM Thermometers5 3. Summary of Method 3.1 A known volume of liquid is spread on a known area of filter paper that is suspended from a sensitive balance in a 1 These test methods are under the jurisdiction of ASTM Committee D-I on Print and Related Coatings and Materials and are the direct responsibility of Subcommittee D0L.24 on Physical Properties of Liquid Paints and Paint Mate rials. Current edition approved May 29, 1987. Published July 1987. Originally Published as D 3539 - 76. Last previous edition D 3539 - 76. 2 These test methods are essentially the same as the one developed by the New York Society for Paint Technology. The Precision section was added by ASTM Subcommittee DO 1.24 and is based upon the data of the New York Society for Paint Technology. 3 See "Comparative Evaporation Kates of Solvents: II," New York Club, Technical Subcommittee No. 66, Official Digest, 28, No. 382, 1956, p. 1060. 4Annual Book ofASTM Standards, Vot 15.05. 5 Annual Book ofASTM Standards, VoLs 05.03 and 14.03. cabinet. Dried air or nitrogen at 25C is passed through the cabinet at a known rate. The loss of weight of the filter paper/liquid is determined and plotted against time. 4. Significance and Use 4.1 The rate of evaporation of volatile liquids from a solution or dispersion is important because it affects the rate of deposition of a film and flow during deposition, and thereby controls the structure and appearance of the film. In the formulation of paints and related products, solvents are chosen based on the evaporation characteristics appropriate to the application technique and the curing temperature. METHOD A--EVAPORATION RATE USING THE MANUAL THIN-FILM EVAPOROMETER 5, Apparatus 5.1 Evaporometer, thin-film evaporometer6 as shown in Fig. 1. 5.2 Constant-Temperature Cabinet for evaporometer. N' 1--Precaution: In instances with the solvents and other volatile materials normally tested using this apparatus and under the conditions specified in this method, the concentration of solvent or other flammable material being exhausted into the laboratory atmos phere will be significantly below any concentration that could be hazardous, that is, a lower flammable limit However, it may be desirable to locate the instrument and cabinet in a laboratory exhaust hood if the routine handling of certain materials may present a hazard due to toxicity, extreme volatility, or flammability. 5.3 Interval Timer: Stop Watch or Electric Timer--A timer that gives an audible signal at 10 or 20-s intervals and that gives a warning signal approximately 3 s before the end of the interval is preferred. 5.4 Filter Paper Disk--Fast, open-texture filter paper, 90 mm in diameter, with a circle approximately 60 mm in diameter (and concentric with the edge) lightly drawn on the paper with a pencil. 5.5 Syringe--A 1,00-mL hypodermic syringe equipped with a 9-in. (225-mm) needle of 0.050-in. (1,3-mm) outside diameter stainless steel tubing.7 Due to manufacturing vari ations, the syringe should be calibrated before use. 5.6 Dehumidification Equipment--A suggested setup is given in a schematic diagram. Fig. 2. 6 The manual Shell thin-film evaporometer is no longer available. 7 Syringe: Becton, Dickinson and Co., No. 1YT available from Fisher Scientific Co. Needle: Special Syringe Needle Type LNR, 18 gage, 9 in. long blunt round end, no bevel-available on special order from Becton, Dickinson and Co. through Fisher Scientific Co., 711 Forbes Ave., Pittsburgh, PA 15239. 521 DUP050297702 D 3539 FIG. 1 Details of the Thin-Film Evaporometer N' 2--Precaution: Use of this dehumidification apparatus re quires the safety practices relative to the handling, use, and disposal of hazardous acids and caustics be observed. When handling these mate rials, protective eye or face, or both, shields and protective clothing arc recommended. N' 3--In those instances where dry nitrogen is available it may be used directly instead of air and thus eliminate the dehumidification equipment The use of nitrogen does not alter the evaporation rate. 5.7 Hygrometer (or other humidity-sensing device), ca pable of indicating low humidities. 5.8 Thermometers, of suitable accuracy such as ASTM Bomb Calorimeter thermometer 56C having a range from 19 to 35C, subdivisions 0.02C or Thermometer 56F (66 to 95F with 0.0SF subdivisions), and conforming to the requirements of Specification E 1. 6. Preparation of Evaporometer 6.1 Place the filter paper disk on the wire support, threading the hook through a small hole in the center of the paper. Attach the hook to the steel spring below the sighting disk and allow the paper and the paper support to hang therefrom. 6.2 Close the evaporometer and cabinet doors and allow the temperature in both chambers and the humidity to equilibrate at the following test conditions: Cabinet and evaporation temperature: 77 0.5F (25 0.25'C) Evaporometer humidity: 0 to 5 % relative humidity Approximately 2 h are required for the humidity to drop to less than 5 %. 6.3 Adjust the air flow to 21 L/min (center of ball float opposite correct mark on the rotometer scale). suit i the i no 9- 7. Conditioning 7.1 Bring the sample or a portion of it to an equilibrium temperature of 77 1.0F (25 0.5C) in a constanttemperature bath. Determine the specific gravity of the sample at this temperature in accordance with Test Methods D 891. i: 8. Procedure 8.1 Record the position of the filter paper as indicated by alignment of the sighting disk with its mirror image. This is the no-load position. 8.2 Raise the wire mesh bracket until the bottom of the disk support rests lightly on it. 8.3 Withdraw into the syringe 0.70 mL of the solvent which is at 77 1.0'F (25 0.5C). Make certain that all air bubbles are expelled from the syringe and the needle before application of the specimen to the filter paper. 8.4 Insert the hypodermic needle into the small opening on the right-hand side of the instrument and position the needle tip so that it almost touches the disk and is just oven the line that was drawn. Ml 8.5 Start applying the solvent to the disk. As the first drop p hits the disk, start the timer. The solvent should be applied at a uniform rate in 2 s and as evenly as possible along the drawn line. To ensure consistent specimen size, touch the tip 1 of the hypodermic needle to the filter paper to dispense the 4 last drop of solvent 8.6 Immediately lower the wire mesh bracket away fromA t]the disk support. Obtain the first reading of the position of the sighting disk at 40 s and then every 20 s. Record the time and the scale reading on the report form. A sample report form is shown in Annex A2. N' 4--With very slow evaporating solvents, it is not necessary to i ; wl 5 El C S V D B Z N se tk fc n> r c \ s 1 AIR IN GAUGE 9 -tsi DIAPHRAGM REGULATOR ROTOMETER, i EVAPOROMETER,! j a I e if ( ] TRAP (GLASS WOOL) H2 Sq4 (95%) H2 So , TRAP NaOH (95%) (GLASS FLAKCS WOOL) N' --One-litre flasks should be used throughout. FIG. 2 Diagram of Dehumidification Apparatus AMHYMOUS Co. So* i ( < i 522 DU PO 502 97703 0.25'C) drop to ill float librium -nstantof the lethods ated by This is of the solvent tall air before pening on the st over st drop jlied at mg the the tip lse the y from tion of le time report sary to nine a ETER # D 3539 ^table time interval after the first 200 s. 8.7 Stop the timer when the sighting disk has returned to original unloaded position. M' 5--The filter paper may be reused provided the solvent leaves #0 appreciable residue in evaporating. 9. Calculation 9.1 Calculate the evaporation rate as follows: ER = O x 100(5 - Z) tfhere: S = Vx DaMZ= N-{S[Q gR = evaporation rate, wt %, C = spring constant, g/crn elongation, 5 = specimen weight, y = 0.70 mL aliquot volatile liquid at 77 i/T.O'F (25 0.5"C), D = density of volatile liquid at 77 1.0F (25 0.5C) (Taken as equivalent to specific gravity but with units of g/mL) g = scale reading taken during evaporation of aliquot, Z = zero percent evaporated, scale reading = N - (S/Q. and R -- no-load scale reading (100 % evaporated reading). 9.2 Plot the percent evaporated against elapsed time in seconds and draw a smooth curve through the points. From the curve, determine at 10 weight % increments to 90 % and for 95 and 100 % evaporation the time in seconds to the nearest value as follows: Approximate Elapsed Time to 100 % Evaporated Point, s Report to Nearest Indicated Value, s Less than 300 300 to 600 600 to 1800 1800 to 3600 3600 to 7200 More than 7200 1 5 10 30 60 nearest 2 % of indicated value N' 6--The curve drawn through the various points should pass through zero or the origin. If it passes to the right of the origin, the delivery time was in excess of 12 s or an aliquot larger than that specified was delivered. If it passes to the left of the origin, then the aliquot was smaller than specified. 10. Report 10.1 Report the elapsed time in seconds at 10 weight % intervals through 90 % and for 95 and 100 % evaporation, and the relative evaporation rate (-butyl acetate = 1.0). Relative evaporation rate is calculated from the 90 weight % evaporated times for the test solvent and for n-butyl acetate (99 % ester). 11. Precision8 11.1 On the basis of an interlaboratory study of the test method in which operators in six laboratories determined the 90 % evaporation point of six solvents covering a broad range in evaporation rate, the between-laboratories coeffi cient of variation was found to be 6.3 % relative at 24 degrees 8 Supporting data are available from ASTM Headquarters. Request RR:D01-1003. of freedom after discarding two divergent values. On the basis of the results obtained by three laboratories on three of the solvents having 90 % evaporated times of 200 to 600 s, the within-laboratory coefficient of variation was found to be 0.83 % relative at 18 degrees of freedom. Based on these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 11.1.1 Repeatability--For solvents with 90 % evaporation times of 200 to 600 s, two results, each the mean of two determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 2.5 %. 11.1.2 Reproducibility--Two results, each the mean of two determinations, obtained by operators in different labo ratories should be considered suspect if they differ by more than 18.2 %. METHOD B--EVAPORATION RATE USING THIN-FILM EVAPOROMETER, AUTOMATIC RECORDING 12. Apparatus 12.1 Evaporometer, Automatic Thin-Film Evaporometer,9 as shown in Fig. 3. 12.2 Filter Paper Disk--See 5.4. 12.3 Syringe--See 5.5. 12.4 Dehumidification Equipment--See 5.6. 12.5 Strip Chart Recorder--Any strip chart recorder ca pable of recording the output signal (0 to 15 mA) from the electronic optical weight-sensing device. The recorder should provide a range ofchart speeds including lA to 2 in. (6.3 to 50 mm)/min. It is also desirable for the recorder to accommo date 2 or more mA ranges in order to regulate the sensitivity of measurement. 13. Preparation of Evaporometer 13.1 Place the filter paper disk on the wire frame threading the hook through a small hole in the center of the paper. Attach the wire frame to the support hook in the evaporometer. 13.2 Close the evaporometer and cabinet doors and equil ibrate both chambers as in 6.2. 13.3 Adjust the air flow to 21 L/min. 14. Conditioning of Sample 14.1 See 7.1. 15. Procedure 15.1 When all components (including the filter paper in place) are at equilibrium, adjust the recording pen to a prominent "zero" position near the edge of the chart on the recorder; then turn the switch for the chart motor to the OFF position. This constitutes the "zero" load and time position for the test. ' The automatic Shell thin-film evaporometer. Apparatus Catalog No. FI522 is available from the FLC Instruments, Inc., 2055 Comprehensive Drive, Aurora, IL 60505. Another evaporometer, the Arizona Instrument EV-l, is available (Arizona Instrument Coip., 2078 East University Drive, Tempe, AZ 85281-4098). Precision data is not yet available, but the instrument operates in the same manner as that described in this test method and is reported to give similar results. 523 DUP0502 97704 # D3539 Area Evapora srssK' 0 mL n = IE g cm2 " \ enC -! |(ecific gravity 3 % evaporat 3 % evaporai lUltipticand, A fractions. fecision8 ! On the ba FIG. 3 Automatic Thin-Film Evaporometer A1 N' 7--The milliampere range and chart speed should be selected, if possible, so that the dimensions of the weight and time axes of the plotted curve are approximately the same length. 15.2 Measure 0.70 mL of test sample into the hypodermic syringe (see 8.3). 15.3 Open the small side door on the right hand side of the insulating cabinet and insert the hypodermic needle through the rubber porthole until the needle tip almost touches the disk and is just over the penciled line. when the recording pen returns to 99.5 % of the original displacementi l.l Remov 16. Calculations and Reporting ith a small 16.1 Determine the evaporation time in seconds at 10) i again sust weight % increments to 90 %, and for 95 to 100 % from the) evaporation curve as follows: ; position of analytical 16.1.1 Divide the theoretical recording pen displacement; [n record \ for the total specimen into ten equal units along the weight) stant, C, * axis of the evaporation curve; then project the established! idedby th' 10 % divisions to corresponding intersecting points on the N' 8--Care must be exercised to avoid depressing the plunger of the syringe during this operation. Otherwise the solvent will be acciden tally and prematurely dispensed onto the paper before the strip chart recorder is started. evaporation curve. The 0 % evaporated or full-load point' ajj| zero time can be obtained either by extrapolation of the! evaporation curve back to zero evaporation time or calcula-i tion using the weight of the sample and the calibration data 15.4 When all is ready turn the strip chart motor switch to the ON position and simultaneously start distribution of the specimen onto the filter paper. The complete specimen should be dispensed uniformly in 10 2 s along the line. The recorder pen will "advance" immediately to an "apex" position equivalent to the total weight of the specimen, less that portion that evaporated dining the application period. The pen will gradually return to its original position as the solvent evaporates and the chart advances. The evaporation is complete when the recording pen has returned to its original "no-load" position. N' 9--It is common for the final portion of the curve to exhibit a "tailing-off." This is due to artifacts of the method such as (1) hydrogen bonding of the last traces of solvent with the cellulose fibers of the filter paper and (2) a gradual diminution of the area of the filter paper wet by solvent (that is, in the final stage of evaporation, drying of the paper progresses from the outer edge toward the center of the disk). Thus, it is common practice for the evaporation cycle to be considered "complete" for the instrument (See Annex A3). The routine calculation*) of the 0 % evaporated, full-load point is recommended as a check for correct specimen size. 16.1.2 Multiply the distance along the time axis from the zero starting time by the chart speed factor in seconds giving the total elapsed time for each defined point along the curve. For example, at a chart speed of 1 in./min and a 20 % evaporation point at 3.30 in. the evaporation time is 198 s (60 X 3.30 = 198). Use the procedure given in 9.2 to round results. 16.2 An alternative method of reporting evaporation results is to express an Area Evaporation Rate, in terms of grams evaporated per second per square centimetre of evaporating surface. ,11115 method is not exact .because the evaporation rate is not linear throughout the complete evaporation period, but it is a useful approximation to represent the general volatility of a solvent. The calculation of evaporation rate is as follows: 524 DUP0502 97705 D3539 Area Evaporation Rate, R = --C--x D-- X 108 ^iiere: g = evaporation rate, g/cm2s x 108, q *= a factor = 0.00438 mL/cm2 obtained from: 0.70 mL = specimen size, 0.80 = increment between the 10 % and 90 % evaporation points (the first and last 10 128 cm2 % increment are disregarded), = total evaporating surface of 90-mm di ameter filter paper, then C = ' 71280'8" = 0.00438 mL/cm2 C = specific gravity of the solvent at 77F (25Q, i = 90 % evaporation time, s, and g = 10 % evaporation time, s. The multiplicand, 10s, is inserted in the equation to avoid decimal fractions. 17. Precision8 17.1On the basis of an interlaboratory study of the test method in which operators in four laboratories determined the 90 % evaporation point of seven solvents covering a broad range in evaporation rate, the within-Iaboratory coef ficient of variation was found to be 1.78 % relative at 35 degrees of freedom and the between-laboratories coefficient of variation was found to be 3.88 % relative at 28 degrees of freedom. Based on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 17.1.1 Repeatability--Two results, each the mean of two determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 5.1 %. 17.1.2 Reproducibility--Two results, each the mean of two determinations, obtained by operators in different labo ratories should be considered suspect if they differ by more than 11.25%. 18. Index Terms 18.1 These test methods are indexed under the following terms: evaporation rate. Shell thin film evaporometer, and evaporation rates of solvents. cement. at 10 :>m the :ement weight olished on the >int at >f the lculai data lation i as a :m the giving curve. . 20 % ; 198 s round >ration rms of :tre of lse the mplete ion to rlation ANNEXES (Mandatory Information) Al. CALIBRATION OF THE THIN-FILM EVAPOROMETER, MANUAL RECORDING Al.l Remove the filter from its wire support and replace it with a small piece of aluminum foil, about 50 by 50 mm; then again suspend the support from the coil spring. Record the position ofthe sighting disk. Load the spring by placing a 1-g analytical balance weight onto the aluminum foil and again record the elongation of the spring. Thus, the spring constant, C, in grams per centimetre, is equal to 1.000 g divided by the elongation in centimetres. A 1.2 Standardization of the Evaporometer--Since there may be slight variations in manufacture, the evaporometer should be standardized prior to routine usage. The standard solvent, rt-butyl acetate, (99 % ester), should have a 90 % evaporation time of 470 10 s under the prescribed test conditions. If the evaporation time is outside these limits, a slight increase or decrease of the air flow should be sufficient to bring about the desired results. 525 DUP0502 97706 D 3539 A2. SAMPLE EVAPORATION RATE REPORT FORM A2.1 A sample evaporation rate report form is shown in Table A2.1. TABLE A2.1 Evaporation Rate Report Form No______________ - Specimen Spring No------------- .; Specimen Volume/ V,. Spring constant, C,--------------------------- g/cm Elongation: Specimen Density/ D, _ No-Load Scale Rearing, N,---------------- _____________ cm; Specimen Weight, S VxD, Zero S-Scale Reading, Z = (N -- (S/C)) Spring Elongation, S/C_ Calculattoh: weight percent Evap. = - x 100 (B-Z) Evaporometer Temperature_ Relative Humidity_______ _ Cabinet Temperature______ _ Date. A Measured at 77 1.0F (25 0.5C). TIME, S SCALE READING (B) SCALE READING (B-Z) SPECIMEN EVAPORA TION %m TIME, S SCALE READING (B) SCALE READING (B-Z) -mi SPECIMEN EVAPORA TION %(W) A3. CALIBRATION OF THE THIN-FILM EVAPOROMETER, AUTOMATIC RECORDING A3.1 The total deflection of the recording pen in chart units divided by the weight added corresponds to the sensitivity of the apparatus. For example, if the total pen deflection is 60 chart divisions for a 0.500-g weight, the sensitivity factor is 120 chart divisions per gram. This value can then be used to establish the 100 % specimen load at "zero" evaporation time and to calculate the percent evapo rated at various time intervals. For instance, pure n-butyl acetate (99 mol %) has a density of 0.878 at 250C, so a 070-mL specimen at the cited calibration would deflect the pen 73.75 chart units (that is, 0.878 X 6.70 X 120 = 73.75). Each 10 % increment that evaporates corresponds to 73.75 chart divisions. } . A3.2 Standardization of the EVapdrometer--Since there may be slight unavoidable variations in manufacture, the evaporometer should be standardized prior to routine usage. Normal butyl acetate (99 % ester) should have a 90%. evaporation time of 470 10 s under the prescribed test, conditions. If the evaporation time is outside these limits, a: small adjustment should be made to the position of the inlet air (or nitrogen) ports within the inner chamber of the evaporometer. Chution: The air should not be directed above or onto the filter paper. acetone Amyl ace Amyl aa Amyl ale jert-Amy penzene isobutyl p-Butyl /t-Butyl sec-But isobuty o-Butyl sec-Bu isobuty Butytl* Cydoh Cydoh pEGM DEGV "' { "' { ( Diace Die*' Diisot Dime Ethyl Ethyl Ethyl Ethy' Ethy Ethy Ethy Ethy Ethy Eth' EGt EGt EGI EG EG s EG 2-E 2-E Et A4. EVAPORATION RATES OF VOLATILE MATERIALS A4.1 The evaporation values presented in Table A4.1 are typical of commercial materials. Deviations from the values shown can be expected due to normal variations in test conditions and purity, composition, source, etc. of test samples. H fi ls tv K K N L N \ L K t t i$ i i 526 DUP050297707 --------------- -mL - - -- -- ------------- - 'ECIMEN 'APDRA- Is to 73.75 lince there icture, the tine usage. e a 90% cribed test >e limits, a :f the inlet jer of the cted above , of test acetone Pinyl acetate (ex. Fusel oil) (85 to 88 X) pjr\<p\ acetate, primary, (mixed Isomers) (95 %) ^iriyl alcohol, primary (mixed isomers) (art-Amyl alcohol Benzene Isobutyl acetate n-Butyl acetate (90 X) rt-Butyl acetate (99 X) sec-Butyl acetate (90 X) Isobutyl alcohol n-Butyl alcohol sse-Butyl alcohol Isobutyl isobutyrate Butyl lactate Cycfohexanol Cyclohexanone OEGMBE OEGMBE acetate "' { 9 ' ' OEGMME Diacetone alcohol Diethyl ketone Dlisobuty! ketone Dimethyl fonmamide Ethyl acetate (85 X) Ethyl acetate (95 %) Ethyl acetate (99 X) Ethyl alcohol (95 X) Ethyl alcohol (100 X) Ethyl amyl ketone Ethylbenzene Ethyl butyl ketone Ethyl ether Ethylene glycol ' { 9 ' ' EGMBE acetate EGMEE EGMEE acetate (95 X) EGMEE 8 acetate (99 X) EGMME8 2-Ethyl hexanol 2-Ethyl hexyl acetate (95 X) Ethyl lactate Hexyl acetate Hexylene glycol n-Hexane Isophorone Mesityl oxide Methyl acetate (80 %) Methyl alcohol Methyl amyl acetate (95 X) Methyl ethyl ketone Methyl isoamyl ketone Methyl isobutyl carbinol Methyl isobutyl ketone Methyl isopropyl ketone Methyl n-amyl ketone Methyl n-propyl ketone 4-Methoxy - 4-methyl pentanone-2 Nitroethane Nitromethane D3539 TABLE A4.1 Evaporation Rates ot Volatile Materials Automatic Evaporometer Seconds to 90 X Evaporation Relative Rate n-Butyl Acetate 1.0 82 690 1 200 2300 505 133 305 460 470 260 740 1 080 585 970 14600 9 200 1 570 150000 328 000 27800 26300 3 840 205 2430 2280 115 117 117 330 280 1 770 562 1 080 40 6 780 14300 1 210 2 700 2 520 880 25700 13400 2580 2 560 SO 20 000 535 93 220 1 000 121 1020 1710 280 164 1 380 200 295 445 360 5.7 0.68 0.39 0.20 0.93 3.5 1.5 1.0 1.0 1.8 0.64 0.44 0.83 0.48 0.03 0.05 0.30 0.01 0.01 0.02 0,02 0.12 2.3 0.19 0.21 4.1 4.0 4.0 - 1.4 1.7 0.27 0.84 0.44 11.8 0,01 0.07 0.03 0.39 0.17 0.19 0.53 0.02 0.04 0.18 0.18 0.01 7.8 0.02 0.88 5.0 2.1 0.47 3.9 0.46 0.27 1.7 2.9 0.34 2.4 1.6 1,1 1.3 Manual Evaporometer Seconds to 90 X Evaporation Relative Rate8 n-Butyl Acetate = 1.0 75 680 1 110 430 6.0 0.65 0.41 0.3 1.0 305 1.5 450 1.0 241 640 1 010 490 980 13600 1 720 1.9 0.70 0.45 0.92 0.46 0.03 0.1 0.26 0.01 0.01 4 320 179 2 460 2400 110 108 100 0.01 0.10. 2.5 0.18 0.19 4.1 4.2 4.5 2 040 1 020 6.22 0.44 8100 13 300 1280 2 820 2 520 2 490 2400 0.06 0.03 0.36 0.16 0.18 0.01 0.03 0.18 0.19 27 600 555 93 220 900 112 1 040 1 790 277 1 250 0.02 0.81 4.8 2.0 0.50 4.0 0.43 0.25 1.6 0*36 390 12 330 1.4 527 DUP05 02 97708 D3539 TABLE A4.1 Continued Automatic Evaporometer Manual Evaporometer 1-Nitropropane n-Octane Isopropyl acetate (95 %} n-Propyl acetate Isopropyl alcohol n-Propyl alcohol Propylene glycol Isopropyl ether Tettahydrofuran Toluene Water Xylene Seconds to 90* Evaporation 645 295 134 220 320 530 57 97 235 1 290 610 Relative Rate n-Butyi Acetate = 1.0 0.73 1.6 3.5 2.1 1.5 0.89 0.01 8.2 4.8 2.0 0.36 0.77 Seconds to 90% Evaporation 600 125 197 290 450 90 229 620 Relative Rate8 n-Butyl Acetate = 1.0 0.75 3.8 2.3 1.6 1.0 5.0 2.0 0.73 * These data are based on tests made with commercial grade n-butyi acetate containing 90 % ester. 8 Key--EdMME, Ethylene glycol moncmethyl ether (2-methoxy ethanol), EGMEE, Ethylene glycol monoethyl ether (2-ethoxy ethanol), EGMBE, Ethylene gtyca monobutyl ether (2-butoxy ethanol), DEC3MME, Diethylene glycol monomethyl ether, DEGMEE, Diethylene glycol monoethyl ether, DEGMBE, Diethylene glycol monobutyi ether. The American Society for Testing and Materials takes no position respecting tlie validity ofanypatent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Yourcomments are Invitedeither forrevision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1. de lea bu at ch; re: M sa re Pr bi Sti 2. 3 d e tl o. vt a c< 4 (i 528 DUP0502 97709 Designation: D 3618 -,85a (Reapproved 1991) Standard Test Method for Detection of Lead in Paint and Dried Paint Films1 This standard is issued under the fixed designation D 3618; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. (i N ' --Keywords were added editorially in July 1991. thylene glycol 'coi monobutyi 1. Scope 1.1 This test method is intended as a screening test to determine if the solids in a paint contain more than 0.5 % lead. The test described barely detects the presence of 0.4 % but gives a definite positive result at the 0.5 % level. N' 1 --This test method may be used to detect the presence of lead at concentrations higher or lower than 0.5 % by making appropriate changes in the specimen size and reagent quantities specified. 1.2 Paints giving an unexpected positive or questionable result should be analyzed quantitatively for lead, using Test Method D 3335. 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. Specific hazard statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings3 D 3335 Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy3 3. Summary of Test Method 3.1 The sample of liquid paint or dried film is prepared by dry ashing a weighed specimen at 475 to 500C. The ash is extracted with hot sodium hydroxide solution and a drop of the extract is transferred to filter paper. Lead present is oxidized to lead peroxide with bromine water, then treated with "tetrabase" to produce a blue quinoidal salt. Known amounts of lead are added to standard paints that are concurrently tested to provide a base for comparison. 4. Significance and Use 4.1 The permissible level of heavy metals in certain 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 31 and Sept. 27, 1985. Published November 1985. Originally published as D 3618 - 77. Last i- evious edition D 3618 -77 (1984). Annual Book ofASTM Standards. Vols 06.03 and 11.01. * Annual Book ofASTM Standards, Vol 06.01. coatings is specified by governmental regulatory agencies. This test method provides a fully documented procedure for determining low concentrations of lead present in both water and solvent-reducible coatings to determine compliance. 5. Apparatus 5.1 Burner, Meker-type. 5.2 Crucibles, porcelain, high-form, 15-mL, with covers. 5.3 Filter Paper, ashless, medium texture. 5.4 Hot Plate, with variable surface temperature control over the range from 70 to 200C. 5.5 Muffle Furnace, maintained at 475 25C. 5.6 Syringe, glass, 2-mL. 5.7 Volumetric Flasks, 50, 100, 1000-mL. 5.8 Paint Shaker. 5.9 Paint Draw-Down Bar. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests unless otherwise specified. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determi nation. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent grade water conforming to Type II of Specification D 1193. 6.3 Acetic Acid, glacial. 6.4 Ammonium Hydroxide (1+1)--Mix 1 volume of concentrated ammonium hydroxide (NH4OH, sp gr 0.90) with 1 volume of water. 6.5 Bromine Water, saturated. 6.6 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 6.7 Lead Standard Stock Solution, Aqueous (1 mg/mL)-- Dissolve 1.600 g of lead nitrate (Pb(N03}2) in 100 mL of water, add 2 mL of nitric acid (sp gr 1.42), and dilute to 1 L. 6.8 Lead Standard Working Solution, Aqueous (0.2 mg/ mL)--Pipet 10 mL of the aqueous lead standard stock 4 "Reagent Chemicals, American Chemical Society Specifications." American Chemical Soc., Washington, DC. For suggestions on the testing of reagents- not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." 529 DUP050297710 # D 3618 solution into a 50-mL volumetric flask and dilute to volume with water. 6.9 Toluene, technical grade. 6.10 Lead Standard Stock Solution, Solvent-Based (1 mg/mL)--Dissolve 4.2 g of lead naphthenate (containing 24 % lead) in LOO mL of toluene and dilute to 1 L. N' 2--Other toluene-soluble lead driers such as lead tallate, lead linoleate, and lead octoate may also be used provided that the lead content is accurately known and the appropriate weight is diluted to 100 mL to provide a toluene solution containing l mg/mL of lead. 6.11 Lead Standard Working Solution, Solvent-Based (0.2 mg/mL)--Pipet 10 mL of the solvent-based standard stock solution into a 50-mL volumetric flask and dilute to volume with toluene. 6.12 Sodium Hydroxide Solution (12 % w/v)--Carefully dissolve 12 g of sodium hydroxide in 100 mL <5f water. 6.13 Paint, Standard Solvent-Reducible, any solvent-re ducible paint known to contain less than 100 ppm of lead. 6.14 Paint, Standard Water-Reducible, any waterreducible paint known to contain less than 100 ppm of lead. 6.15 Tetrabase Reagent (4,4'-Methylenebis (N,N-dimethylaniline)), l % in 10 % Acetic Acid--Dissolve 1 g of tetrabase5 in 50 mL of water to which 10 mL of glacial acetic acid has been added. Dilute to 100 mL with water. 7. Hazards 7.1 Glacial acetic and concentrated nitric acids will cause burns of the skin and eyes. Sodium hydroxide is corrosive. Use care in handling these materials. Avoid contact with skin. Refer to suppliers' Material Safety Data Sheets. Bro mine water should be prepared and used in a laboratory hood.6 7.2 Use only a rubber bulb aspirator for pipetting liquids. 8. Procedure 8.1 If the sample is a liquid coating, mix it until homoge neous, preferably on a mechanical shaker. Determine the nonvolatile content in accordance with Guide D 2832. N' 3--Recover dried paint films from previously coated sub strates (being careful not to remove any underlying material from the substrate) or prepare in the laboratory from liquid samples. For the laboratory preparation, flow some ofthe well-mixed sample onto a clean glass plate. The use of a paint draw-down bar is recommended to obtain a uniform dim thickness not exceeding 2 mils (50 pm). Allow to dry in an oven at 105C for a minimum of 1 h. Scrape the dried film off the glass plate, preferably with a single edge razor blade. 8.2 Weigh to 0.1 mg, 50 mg of paint solids into a porcelain crucible or 50-mL glass beaker. For a liquid coating, determine the specimen weight to be taken by the following equation: where: S' = specimen weight, g, and C = nonvolatile content, % 5 Eastman-244 (Eastman Organic Chemicals, Rochester, NY 14650) has been found to be satisfactory, equivalent grades may be used. * Saturated bromine water may be purchased from chemical supply houses. N' 4--Crucibles or beakers used in this test method should k, new or in very good condition. Otherwise, it is possible that some ]Lj may be lost and a false negative obtained. J 8.3 Weigh 50 mg of solids from the appropriate standard paint (solvent-reducible or water-reducible) into each of tw0 additional porcelain crucibles or 50-mL glass beakers. Usk a 2-mL glass syringe, add 1.0 mL of the appropriate 200-pp^j standard working solution (solvent-reducible or water-re. ducible) to one of the crucibles or beakers, and 1.8 mL to thP other. N' 5--The standard paint to which has been added 1.0 ml 0f standard working solution contains approximately 0.4 % lead based 0n the paint solids, and the one to which has been added 1.8 mL of standard working solution will contain approximately 0.72 % lead based on the paint solids. 9 1 9 exet pen , 10. li ' 7 <, poi- 8.4 Place all three crucibles or beakers on a cold hot plate and slowly increase the temperature until the material jj dried. With some types of coatings, an initial oven-drying at 105C may be necessary to remove solvents without incurring losses due to spattering. 8.5 When the specimens appear to be dry, or when starting with a dried film, gradually increase the temperaturt of the hot plate until the material chars. 8.6 After charring is complete, place the crucibles or beakers in a preheated muffle furnace and ash at 475 to 500'C. 8.7 When the ashing appears to be complete, (approximately 1 to 2 h) remove the crucibles or beakers from the muffle furnace and allow them to cool to room temperature. Add 5 mL of 3 N sodium hydroxide solution to each crucible or beaker and mix thoroughly with a stirring rod. Scrape any adhering residue from the sides or bottom of the container and break up any particles, using a separate stirring rod for each specimen. 8.8 Place covers on the crucibles or watch glasses on the beakers, and boil gently for approximately 5 min. Remove from the hot plate and allow the contents to settle. Do not fdter. 8.9 With the tip ofthe stirring rod, transfer 1 to 2 drops of each extract to the center of a piece of filter paper. Using separate droppers, successively apply directly on each spec imen spot a drop of bromine water and a drop of NH4OH solution. Remove excess ammonia by holding each filter paper over a hot plate until no odor is detectable, but do no! take to complete dryness. Place 2 drops of tetrabase reagenti on each spot and compare the color developed on the specimen spot with those on the standard paint spots. To f ensure that maximum color development has been achieved, add I or 2 more drops of tetrabase reagent on the center of each spot after the first addition has almost-dried (if still wet the color may diffuse). N' 6--Although the color is stable, it is barely visible in the rangf i from 0.4 to 0.5 %. Comparing results with those obtained on the two standard paints helps to orient the observer to the color intensity to h ; expected. N' 7--Certain iron-based pigments have high natural manganes : levels. The ash extract of products containing high manganese ma) produce a diffuse blue ring on the filter paper. With experience, this 8 easily distinguished from the small blue spot produced by lead. -5--3-0----------------------------------------- ----------___ DUP050297711 should b'e some lead standard :h of two rs. Using 200-ppm water-renL to the 1.0 mL of 1 based on 1.8 mL of lead based hot plate aterial is drying at ut incur- or when iperature dbles or t 475 to 'approxifrom the perature. i crucible :rape any :ontainer g rod for :s on the Remove . Do not irops of . Using :h spec'-IH4OH :h filter at do not e reagent l on the .pots. To achieved, center of ' still wet, 1 the range >n the two nsity to be manganese anese may nee, this is id. # D 3618 9. Report 9.1 Report a positive test (lead content equal to or in excess of 0.5 % of paint solids) when a blue color forms and persists for several seconds. 10. Precision and Bias7 10.1 An interlaboratory test was conducted in which 'Supporting data are available from ASTM Headquarters. Request RR: pOl-1007. analysts from eight laboratories tested water and solventbased coatings having lead contents slightly lower and slightly higher than 0.5 % based on the solids. All analysts made correct judgments for greater than 0.5 % lead (positive) and less than 0.5 % lead (negative), with only one analyst reporting a single result as "questionable." 11. Keywords 11.1 lead; lead in paints and dry paint films; spat test for lead The American Society for Testing and Materials takas no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at anytime by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision oi this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel thet your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 531 DUP050297712 I1 Designation: D 3623 - 78a (Reapproved 1987) plate per Sp to 12 in. (31 Standard Method for Testing Antifouling Panels in Shallow Submergence1 vvith a mini(6-mm) diai shall be dri painting. T This standard is issued under the fixed designation D 3623; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A substrate f minimum; superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 6.2 Stan coating sys 1. Scope 4, Terminology 6.2.1 Gi 1.1 This method covers a procedure for testing antifouling compositions in shallow marine environments and a stan dard antifouling panel of known performance to serve as a control in antifouling studies. 4.1 Definition: 4.1.1 shallow submergence--an immersion to depths be. tween 1 and 10 ft (0.3 and 3.0 m). 4.2 Abbreviations: Military S revision or 6.2.2 V; Specificati N' --Subcommittee DO1.45 has a revised rating procedure now being evaluated by round robin. 2. Referenced Documents 2.1 ASTM Standards: A 569/A 569M Specification for Steel, Sheet and Strip, 4.2.1 The following abbreviations are used in reporting test results: A1 . algae Barn ' barnacles E.B. encrusting bryozoans Hyd hydroids SI sUme Tun tunicates only. 6.2.3 V tary Sped sion only. 6.3 Te: may be i other suit Carbon (0.15 Maximum Percent), Hot-Rolled, Commer C.F. completely fouled 7. Safetj cial Quality2 D2200 Pictorial Surface Preparation Painting Steel Surfaces3 2.2 U.S. Military Specifications: Standards for F.R. A.F. A.C. O.P. CO fouling resistance rating antifouling rating anticorrosive rating overall performance rating coelenterates 7.1 Cs that cou adverse preparat MIL-P-15328D Primer Pretreatment (Formula 117 for F.B. filamentous bryozoans antifouli Metals)4 Mol molluscs and equ 1 MIL-P-15929C Primer Coating, Shipboard, Vinyl-Red PC polychaetes federal Lead (Formula 119--For Hot Spray)4 4.2.2 Algal Mups may be delineated by classification and ted IS MIL-P-15931B Paint, Antifouling, Vinyl, Red (Formula notation by phyllum as follows: rial sho 121/63)4 Hi MIL-S-22698A Steel Plate, Carbon, Structural4 Al-b Al-bg Phaeophyta (brown) Cyanophyta (blue-green) disposei 3 Al-g Chlorophyta (green) 8. Proc 3. Significance and Use 3.1 This method is designed as a screening test in evalu ating antifouling coating systems. Results of the standard system in a specific marine environment are included to assist in interpreting results. 3.2 Antifouling systems providing positive comparisons with the standard system should be considered acceptable for use in protecting underwater marine structures. 3.3 The degree and type of fouling will vary depending on the environment. Hence, differences in geographic location of test sites, in time of year when panels are exposed, and in Al-r Rhodophyta (red) 5. Apparatus 5.1 Blast Cleaning Apparatus capable of preparing panels in compliance with 8.1. 5.2 Application Equipment consisting of brush, roller, conventional spray, or airless spray. Usually the equipment is dictated by the physical properties of the coating and the film thickness desired. 5.3 Exposure Rack to provide firm positioning of the specimen panels such that they are held vertically in place in spite of the current and are electrically insulated from 8.1 t near-wl profile No t with th (2) Pre surface 8.2 apply coatir of */2 ' weather conditions from 1 year to the next can affect results. metallic contact with the rack or other panels. The rack I Nor Therefore, a fouling census on a nontoxic surface is taken. should be positioned such that the prevailing tidal currents 2TC a For the exposure to be valid the nontoxic surface should will move parallel to the panel face, and the panels will be 8.3 j show heavy fouling, and the standard system should show immersed to a depth of a minimum of 1 ft (0.3 m) and a apply significantly less fouling than the nontoxic surface. maximum of 10 ft (3 m). In a rack where the panels are Appl' stacked front to back, they should be spaced at least 2'h in. nomi ; (60 mm) apart, with the two end positions filled with blank mini i 1 This method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.45 on Marine Coatings. Current edition approved Oct. 27, 1978. Published January 1979. Originally panels. In a rack where the panels are mounted side by side, coats the distance between adjacent panels should be a minimum 8.` >/2 in. (1.5 mm). ; dryii published as D 3623 - 78. Last previous edition D 3623 - 78 2AnnualBook ofASTM Standards, VoI01.03. 6. Materials i first 3 Annual Book ofASTMStandards, Vol 06.01. 4 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia. PA 19111-5094, Attn: NPODS. 6.1 Test Panel--The substrate for the standard antifouling coating system shall be medium low-carbon steel 532 DUP050297713 hs be- cation panels filer, nent 1 the ' the ace in from ; rack .rrents vill be and a ;ls are \'h in. blank y side, imum mdard n steel D3623 late per Specification A 569,5 */s in. thick by 6 to 10 by 10 P 12 in. (3 mm thick by 150 to 250 mm by 250 to 300 mm) a minimum area per side of 72 in.2 (465 cm2). A '/4-in. ^min) diameter hole, V2 to 1 in. from the top and centered hall be drilled for holding the panel while handling and Minting. The test coating system shall be applied to that substrate for which it is designed provided there is a minimum area per side of 72 in.2 (466 cm2). 6.2 Standard Coating System--The standard antifouling coating system shall consist of: 6.2.1 Green pretreatment coating conforming to U.S. Military Specification MIL-P-15328B (Formula 117), B revision only. 6.2.2 Vinyl red lead primer conforming to U.S. Military Specification MIL-P-15929C (Formula 119), C revision 6.2.3 Vinyl antifouling coating conforming to U.S. Mili tary Specification MIL-P-15931B (Formula 121/63), B revi sion only. 6.3 Test Coating System--The test antifouling coating may be applied to the standard primer system, or to any other suitable anticorrosive primer system. 7. Safety Precautions 7.1 Caution--Antifouling paints contain toxic materials that could cause skin and eye irritation on contact and adverse physiological effects if ingested or inhaled. In the preparation of panels and the application of various types of antifouling paints the use of appropriate protective clothing and equipment is required consistent with local, state, and federal government regulations, and recognized industrial and technical standards. Spills, overspray, and unused mate rial should not be flushed down the drain, but should be disposed of as hazardous waste. 8. Procedure 8.1 Abrasive blast the required number of panels to near-white metal (Sa 21/2 of Method D2200) to obtain a profile of 1 to 1.5 mils (25 to 38 pm). N' 1--A profile of 1 to 1.5 mils (25 to 38 pm) can be obtained with the following parameters: (1) Type and size of grit. No. 46 (sand); (2) Pressure, 90 psi (620 kPa); (3) Angle, 90 deg; (4) Distance from surface, 3 to 5 in. (75 to 125 mm); (5) Nozzle size, % in. (9 mm). 8.2 On the clean, dry, uncontaminated, blasted surface apply to each standard panel one coat of pretreatment coating MIL-P-15328D to give a nominal dry film thickness of V2 mil (13 pm). N' 2--All coating drying times are for a minimum temperature of 2lC and a maximum relative humidity of 70 %.. 8.3 Within 24 h of application ofthe pretreatment coating apply the first coat of red lead vinyl primer MIL-P-15929C. Apply a total of four coats of red lead vinyl primer to give a nominal dry film thickness of 6 mils (150 pm). Allow a minimum of 2 h and a maximum of 24 h drying between coats of red lead vinyl primer. 8.4 Allowing a minimum of 2 h and a maximum of 24 h drying after the last coat of red lead vinyl primer, apply the first coat of vinyl antifouling coating MIL-P-15931B to the 5 See also U.S. Military Specification MIL-S-22698, Type 1, Class A. standard panels, and the test coating to the test panels. A 3/4-in. (19-mm) numbered vinyl tape can be applied before the second coat of antifouling coating for identification. Allowing a minimum of 2 h and a maximum of 24 h drying after the first coat, apply a second coat of the respective antifouling coating to give a nominal dry film thickness for both antifouling coats of 4 mils (100 pm). 8.5 Before immersion permit the second coat of antifouling coating to dry a minimum of 4 h and a maximum of 2 weeks, the latter time allowing for shipping the panels to the immersion site. 8.6 Expose for a minimum period of 1 year at an immersion site with a high incidence of fouling as indicated by attachments on a dark nontoxic surface such as slate. A monthly fouling census as well as a yearly accumulation when appropriate is required. 8.7 Evaluate the antifouling panels for surface fouling and physical condition of the film system at least monthly as follows using the report form in Table 1. 8.7.1 Fouling on Surfaces--Rate fouling present on that portion of the antifouling test surface which is intact at the time of inspection (see 9.1). Rate both sides of the panel if appropriate. Ignore fouling present on the substrate or on anticorrosive undercoats. Barnacles, polychaetes, coelenterates, etc., that are immature or loosely attached should be so reported in the appropriate space. Report fouling by initial algal germination, low-form algae and diatoms as "algal slime." Report absorbed organic and inorganic chemicals, trapped silt and detritus, and other unidentified slimes as "silt." 8.7.2 Physical Condition--Rate the condition of coating films in accordance with 9.2. Record qualitative descriptions of film deterioration and discoloration in this column, and unless otherwise specified, refer only to the antifouling test surface. Indicate deterioration of undercoats, when evident, by the notation "A.C.". For example, "Peeling, A.F. from A.C." or "Chipping, A.C. from steel". 9. Calculations: 9.1 Fouling Resistance (F.R.)--Award each test surface free of fouling except for the presence of algal spores and other biological slimes a rating of 100. Reduce the rating to 95 if only incipient fouling is present. If mature forms of fouling are present, obtain the rating by subtracting from 95 the sum of the number of individuals present and percent surface covered by colonial forms. For example, if the "fouling on surface" is: Bam E.B. Others 6, 3 to 10 mm None Mol 1,20 mm Al-g (green) 10 % then the F.R. percent rating would be 95 - (6 + 1 + 10) = 78. 9.2 Physical Condition: 9.2.1 Antifouling Film (A.F.)--Award an antifouling test surface having no physical defects a rating of 100. Subtract the percent surface affected by film defects from 100 to obtain the rating for imperfect films. 9.2.2 Anticorrosive Film (A.C.)--Obtain the rating by the same procedure as 9.2.1. 533 DUP050297714 D 3623 TABLE 1 Behavior Report ol Experimental Surfaces Origin: Series: Base: Size: - Place of Immersion: Depth of Immersion: Date Immersed: Date Inspected: Inspected by: Test Surface No. Fouling on Surfaces'* Bam: E.B.: Others: Physical Condition F.R. Percent Ratings A.F. A.C. O.P, Bam: E.B.: Others: Bam: E.B.: Others: Bam: E.B.: Others: Bam: E.B.: Others: Barn: E.B.: Others: Bam: E.B.: .:*;S Others: Ingrt P< Zi L 6 li V ingi f * The resin 18.0 to 20.0 T gravity of the 0 The zinc c Isopropy " Fouling reported as found on the more heavily fouled surface. Solitary forms reported numerically: colonial forms by percent surface covered, Al: algae: Bam barnacles; E.B.: encrusting bryozoans;; Hyd: hydrolds: Tun: tunicates; C.F.: completely fouled; CO: coelenterates; F.B.: filamentous bryozoans; Mol: molluscs; P polychaetes. 9.3 Overall Performance (O.P.)--For overall perform sure must be included in the report. ance, award the panel the lowest percent rating of the three preceding values. 11. Precision 9.4 Normalization--The rating system described above is 11.1 The precision statements are based on an inter <f '}'M based on a minimum test on one side area of 72 in.2 (465 laboratory study in which seven laboratories prepared pairs ill cm2). Correct the percent ratings for test surfaces of non standard dimensions for the difference between the min of panels coated with the standard antifouling system, submerged them, and after 1 year rated the fouling. The: imum standard panel area of 72 in.2 (465 cm2) and the area within-laboratory standard deviation was found to be 2.08. on one side of the test specimen. 10. Report 10.1 Report the results of the immersion test in terms of The between-laboratory standard deviation was found to be 4.67. Based on these standard deviations, the following criteria should be used to judge the acceptability of results at the 95 % confidence level: Hydr< gravity no 0 To c. cToo fouling resistance and overall performance for both the 11.1.1 Repeatability--Two results each the mean of du material under test and the standard system. plicates obtained by the same operator should be considered 10.2 Other Data--Report the place, depth, and date of suspect if they differ by more than seven units. immersion, whether mounted from a dock or a floating raft, 11.1.2 Reproducibility--Two results each the mean of date the panels were removed and inspected, panel size, and duplicates obtained by operators in different laboratories panel identification number. A census of fouling on a should be considered suspect if they differ by more than 16 nontoxic surface taken each month for the period of expo units. *Thi BTtv of 1.35 Th 534 DUP050297715 03623 ------------ . --------- ---- . ---------- --, Igae; Bam: lluscs; PC: n intered pairs system, ng. The be 2.08. nd to be llowing suits at of dusidered nean of oratories than 16 ANNEXES Al. STANDARD COATING SYSTEM FORMULAS TABLE A1.1 Green Pretreatment Coaling, MIL-P-15328D (Formula 117) Pounds per 100 gal of Mixed Material Gallons per 100 gal of Mixed Material Ingredients of resin component (80 gal): Polyvinyl-butyral rasin'* Zinc chromate (insoluble type)3 Magnesium-silicate (Type AorB of Specification MIL-M-15173) Lampblack (Specification TT-L-70) Butyl alcohol, normal (Spec. TT-B-846) Isopropyl alcohol, 99 %c Water Ingredients of acid component (20 gal): Phosphoric acid (Class A of Spec. O-P-313) Water Isopropyl alcohol, 99 Xc 56 54 8 0.6 125 353 15 28 25 99 6.10 1.78 0.34 0.04 18.48 53.80 1.80 2.0 3.0 15.0 * The resin shall be a polyvinyl partial butyral resin containing only polyvinyl butyral), poly(vinyl alcohol), and poly(vinyi acetate) In the molecule. The resin shall contain 18.0 to 20.0 % vinyl alcohol, and not more than 1.0 % of vinyl acetate. A 6 % solution of the resin in methanol shall have a viscosity of 12 to 18 cP at 20C. The specific gravity of the resin shall be 1.05 to 1.15. The zinc chromate shall be of an insoluble type, showing an analysis of 16 to 19 % Cr03, and 67 to 72 % ZnO, and not more than 1 % water-soluble salts. c Isopropyl alcohol. 99 % shall have a specific gravity of 0.785 to 0.790 at 20/20C and a distillation range not greater than 1.5C and this range shall include 82.3C. TABLE A1.2 Vinyl Red Lead Primer, MIL-P-15929C (Formula 119) Ingredients Specifications Pounds per 100 gal Composition G Composition L Red lead, 9S % Pb30,, Organic suspension agent 24 % NV Vinyl resin* Tricresyl phosphate Methyl Isobutyl ketone Methyl n-butyl ketone8 Methyl ethyl ketone Toluene Aliphatic naphtha0 TT-T-656 TT-M-268 TT-M-261 TT-M-261 TT-T-548 TT-N-95,(I) 247.0 8.2 162.8 16.8 284.7 47.0 217.7 247.0 8.2 162.8 16.8 273.2 105.5 75.1 81.1 A Hydroxyl containing vinyl chloridd-acetate copolymer (89.5 to 91.5 % vinyl chloride, 5.3 to 7.0 * vinyl alcohol and 2 to 4.0 * vinyl acetate): white powder, specific gravity not under 1.35, not less than 98 % through sieve 20. To contain not over 5 volume * of branched chain ketones. 0 To contain not over 11 volume % of aromatic hydrocarbons. TABLE A1.3 Vinyl Antifouling Coating, MIL-P-15931B (Formula 121/63) Ingredients Specifications Pounds* Cuprous oxide Rosin Vinyl resin Tricresyl phosphate Methyl isobutyl ketone Xylene Antisettling agent0 MIL-P-15169 LLL-R-626, Class A, Grade WW TT-T-656 TT-M-286 TT-X-916 1440 215 55 50 165 115 5to9 A The formula given Is slightly in excess of 100 gal to allow for normal manufacturing loss, may be proportioned to the size batch desired. s The resin shall be a vinyl chloride-vinyl acetate copolymer. It shall contain 85 to 88 % vinyl chloride and 12 to 15 % vinyl acetate. The resin shall have a specific gravity of 1.35 to 1.37. Material shall be furnished as a powdered white solid, not less than 98 56 of which shall pass through a No. 20 sieve, conforming to RR-S-366. c The antisettling agent shall be sufficient to prevent hard pigment settfirig and otherwise meet requirements of Military Specification MIL-P-15328D, Section 3.4.6. 535 DUP050297716 I D 3623 A2. RESULTS OF EXPOSURE OF STANDARD ANTIFOULING PANELS I YEAR AT MIAMI BEACH, FLA AT A MINIMUM DEPTH OF I FT (0.3 m) UNDER A FLOATING RAFT N' --Physical condition or its extent indeterminate, or both, due to intensive, extensive algae spore growth. Ratings for A.F. and A.C. are as recorded before surface became obscured by spore foulings. Origin: Series: Base: Size: ASTM Subcommittee 48 #1 Steel 10 by 12 in. and 6 by 12 in. and 8 by 10 in. Place of Immersion: ate Immersed: Date Inspected: Inspected by: Miami Beach 11 June 1971 11 June 1972 F. Lepicard Test Surface No. VAL/1 numbered Bam: incipient E.B.: 2* Others: A1 (green and red) 1% A1 (spores) 85 * Physical Condition soft pinhead blistering (extent indeterminate), see note Percent Ratings F.R. A.F. A.C. O.P. ~ 92 98 100 92 VAL/1 unnumbered Bam: 10,4-7 mm E.B.: 6 % Others: A1 (spores) 85 % soft pinhead blistering (extent Indeterminate), see note - 79 99 100 79 NN/1 numbered Bam: 2,3 to 10 mm E.B.: 14 % Others: A1 (spores) 90 % soft eroding (extent indeterminate), see note 79 98 100 79 NN/1 unnumbered Bam: incipient E.B.: 3 % Others: A1 (spores) 95 % soft (extent indeterminate), see note 92 99 100 92 MMR/1 numbered Bam: none E.B.: 1 % Others: A1 (spores) 30 % eroding 94 90 100 90 MMR/1 unnumbered Bam: Incipient E.B.: none Others: A1 (spores) 50 % eroding 95 95 100 95 VAL/2 numbered Bam: incipient E.B.: 2 % Others: A1 (spores) 80 % indeterminate, see note 93 io'd 100 93 VAL/2 unnumbered Bam: incipient E.B.: 4 % Others: A1 (spores) 80 * indeterminate, see note 91 100 100 91 NN/2 numbered Bam: 4,3 to 6 mm E.B.: 3 % Others: A1 (spores) 85 % Indeterminate, see note 88 100 100 88 ... NN/2 unnumbered Bam: incipient E.B.: 10* Others: A1 (spores) 90 * indeterminate, see note 85` 100 100 86 MMR/2 numbered Bam: none E.B.: none Others: A1 (spores) 45 * Indeterminate, see note 100 100 100 100 MMR/2 unnumbered Bam: none . E.B.: 1% Others: A1 (spores) 40 % ` '-n ' ' indeterminate, see note 94 100 . . 100 94 NLC/1 unnumbered Eiam: none E.B.: 2 % Others: A1 (spores) 85 % Indeterminate, see note 93 100 100 93 NLC/2 numbered Bam: incipient E.B.: 5 * Others: A1 (spores) 65 * Indeterminate, see note 90 100 ,100 90 NLC/2 unnumbered Bam: none E.B.: none indeterminate, see note Others: A1 (spores) 90 % FIG. A2.1 Behavior Report of Experimental Surfaces 100 100 100 100 EPA 171 EPA 171 EPA 271 EPA 271 EPA 371 EPA 371 EPA 471 EPA 471 SW/1 SW/1 SW/2 SW/2 A Foui Bam: Bai 536 DUP050297717 D3623 FIG. A2.1 (Continued) Test Surface No. PA 171 numbered Bam: 9,3 to 11 mm E.B.: 2% Others: A1 (red) 1 % A1 (spores) 80 % Physical Condition Indeterminate, see note Percent Ratings F.R. A.F. A.C. O.P. 83 too 100 83 EPA 171 unnumbered Bam: none E.B.: 4 % Others; A1 (spores) 85 % Indeterminate, see note 91 100 100 91 Barn: none O.P. EPA271 numbered E.B.: none indeterminate, see note Others: A1 (red) 1 % 92 A1 (spares) 90 % Bam: Incipient, EPA 271 unnumbered E.B.; 12 % Indeterminate, see note Others: A1 (green and red) 2% 79 A1 (spores) 80 st EPA 371 numbered Bam: incipient E.B.: 1 * Others: A1 (red) 1 * indeterminate, see note 79 A1 (spores) 80 % Bam: Incipient EPA 371 unnumbered E.B.: 6 55 Indeteimlnate, see note 92 Others: A1 (spores) 95 % Bam: incipient EPA 471 numbered E.B.: 3 % indeterminate, see note 90 Others: A1 (green and red) 2% A1 (spores) 90 % 95 Bam: incipient EPA 471 unnumbered E.B.: 1 % indeterminate, see note Others: A1 (green and red) 1* 93 Al (spores) 65 % 94 100 100 94 81 100 100 81 93 100 100 93 89 100 100 89 90 100 100 90 93 100 10O 93 SW/1 91 numbered Bam: none E.B.: 7% Others: Al (spores) 65 % indeterminate, see note 88 100 100 88 88 SW/1 unnumbered Bam: incipient E.B.: 5 % Others: Al (spores) 75 * . indeterminate, see note 90 100 100 so swy2 85 numbered Bam: incipient E.B.: 2% Others: Al (spores) 90 % indeterminate, see note 93 100 100 93 100 SW/2 unnumbered Bam: none E.B.: none Others: Al (green and red) : 3% Al (spores) 85 % indeterminate, see note 5' 92 100 100 92 94 A Fouling reported as found on the more heavily fouled surface. Solitary forms reported numerically; colonial forms by percent surface covered, At: Algae; An: Anomia; Bam: Barnacles; Bug: Bugula; E.B.: Encrusting Bryozoans; Hyd: Hydroids; Oy: Oyster; Sp: Sponge; T. W.: Tube worms; Tun: Tunicates; C.F.; Completely fouled. Reprinted Courtesy of Miami Marine Research, Inc. 93 90 100 537 DUP050297718 A3. FOULING CENSUS--JUNE 1971 TO JUNE 1972-4 Test Surface: Exposure: Date June 1971 July 1971 Aug. 1971 Sept. 1971 Oct. 1971 Nov. 1971 Dec. 1971 Jan. 1972 Feb. 1972 March 1972 Apr. 1972 May 1972 June 1972 Barnacle Count 209 618 225 2206 1090 1354 983 660 176 726 1120 1618 900 Tube Worm Count 44 24 44 5 none 2 57 157 145 560 560 150 350 Oyster Count 7 9 1 7 50 10 . none 3 none 4 1 7 10 8 by 10 In. Slate (Nontoxic) From raft, 1 ft (0.3 m) beneath water surface Tunicates 70* 65* 95* 55* 20* 5* 2% 5% 5* 5* 10* 10* 20* Hydroids 10* 8* 18* 3* 10* 3* . 15 % 60% 60* 50% 40% 30* 1* Algae 3% . 5% 5* 5% 15* 7* 0% 35* 85* 85% 92% 20* 10% Encrusting Bryozoa 1% 1% 1* none 2% none 3% 6% 3% 40% 25% 1% 1% Bugola 2% 2% none none " none 1% 2% 1% 1% 1% none Reprinted courtesy of Miami Marine Research, Inc, A4. SUMMARY OF BARNACLE SETTLEMENT FOR EXPOSURE PERIOD OF ANNEX A2. BOO 400 ANNUAL SUMMARY OF Over 600 Over. 600 BARNACLE SETTLEMENT @B. Improvisus jggB. Amphitrite ^B.Eburneus HB.Trigonus SSB.Variegatus 1. Sco 1.1 conten (mg/k| dried detem dilutic quant 1.2 safety respa priate 300 BOO ioo JUL AUG SEP OCT NOV DEC JAN FEB MAR APR MAY JUN t------------------- 107*1 -------------------------------1 |------------------------------ 1S7E------------------------------j FIG. A4.1 Summary of Barnacle Settlement. TheAmerican Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ' if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 538 DUP05029771 9 Designation: D 3624- 853 (Reapproved 1991)'61 jgola 1% "* 2% one one one one 1% 2% 1% 1% 1% one one IfC/7, fr?C. Standard Test Method for Low Concentrations of Mercury in Paint by Atomic Absorption Spectroscopy1 This standard is issued under the fixed designation D 3624; the number immediately following the designation indicates the year of original adoption or, in the case of revision, die year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. ei N' --Keywords were added editorially in July 1991. 1. Scope 1.1 This test method covers the determination of the content of mercury in the range between 10 and 1000 ppm (mg/kg) present in liquid coatings, coatings vehicles, or in dried films obtained from previously coated substrates. There is no reason to believe that higher levels could not be determined by this test method, provided that appropriate dilutions and adjustments in specimen size and reagent quantities are made. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user ofthis standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. Specific hazard statements are given in Section 7 and 9.1.1. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water2 3. Summary of Test Method 3.1 The sample of liquid coating or dried film is weighed into a polytetrafluoroethylene (PTFE)-lined acid decomposi tion vessel and digested at an elevated temperature using sulfuric and nitric acids. Use of a sealed acid decomposition vessel prevents loss of mercury during the digestion. The digested sample is diluted to a known volume with water and the concentration of mercury is determined using a coldvapor, atomic absorption technique. 4. Significance and Use 4.1' The permissible level of heavy metals in certain coatings is specified by governmental regulatory agencies. This test method provides a fully documented procedure for determining low concentrations of mercury present in both water and solvent-reducible coatings to determine compli ance. 5. Apparatus 5.1 Atomic Absorption Spectrophotometer--Any commer- , 1 This test method is under the jurisdiction ofASTM Committee D-l on Paint : and Related Coatings and Materials and is the direct responsibility of Subcomjj mittee DO 1.21 oa Chemical Analysis of Paints and Paint Materials. Current edition approved July 17 and Nov. 29. 1985. Published January 1986. Originally published as D 3624 - 77. Last previous edition D 3624 - 84. : 2 Annual Book ofASTM Standards* Vols 06.03 and 11.01. cial instrument having an open sample presentation area in which to mount the absorption cell or an instrument designed specifically for the measurement of mercury using the cold vapor technique. 5.2 Recorder, 0 to 10 mV. 5.3 Mercury Source Lamp. 5.4 Absorption Cell--Standard spectrophotometer cells 100 mm long, having quartz end windows may be used. Prior to use, the cell must be positioned in the optical path of the spectrophotometer and held in place by suitable clamps or straps. The cell should be carefully aligned both vertically and horizontally to give the maximum transmittance. 5.5 Reduction Vessel--Cylindrical gas washing bottle, 250-mL, equipped with a coarse (40 to 60-p.m) fritted glass inlet tube and a standard-taper glass stopper. Polyethylene or poly(vinyl chloride) tubing may be used for connecting the reduction vessel to the absorption cell. 5.6 Flowmeter, capable of measuring a gas flow of 1 L/min. 5.7 Drying Tube--Approximately 6 by 3A-m. (150 by 20-mm) glass tube filled with magnesium perchlorate. The tube should be filled each day that it is in use, and the Mg(C104)2 should be replaced whenever it becomes satu rated (carefully observe after each analysis). N' 1--Use ofan indicator desiccant at the exit end of the tube will make this observation easier. 5.8 Water Vapor Trap--A second 250-mL gas washing bottle (the same as used for the reduction vessel). If pre ferred, a 250-mL Erlenmeyer vacuum flask fitted with a one-hole stopper and 200 mm of 5-mm outside diameter glass tubing, may be substituted. 5.9 Mercury Trap--A. 250-mL Erlenmeyer vacuum flask containing 75 mL of 10 % sulfuric acid and 75 mL of 0.1 N potassium permanganate solution to absorb the mercury vapor after analysis. 5.10 Circulating Oven, maintained at 140 5C. 5.11 Acid Decomposition Vessel, with 25-mL PTFE diges tion cup.3 5.12 Volumetric Flasks, 100, 250, and 1000-mL. 5.13 Paint Shaker. 5.14 Paint Draw-Down Bar. 3 Acid decomposition vessel manufactured by the Parr Instrument Co., 211 Fifty-third St, Moline, IL 61265 (Catalog No. 4745) has been found satisfactory for this purpose. 539 DU P050297720 #-0 3624 until tl 8.5 ,,o add fritted a good detenu ^ blan j-eageh meter, should tion u piaxiir NOT! lyzing 1 diluted - RG. 1 Apparatus the opt this opi volume 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Hydroxylamine Hydrochloride Solution (100 g/L)-- Dissolve 10 g of NH2OH*HCl in 100 mL of water. Transfer a portion of this solution to a small dropping bottle. 6.4 Mercury Solution, Stock (I mg/mL)--Dissolve 0.1354 g of HgCl2 in 50 mL of water. Carefully add 5 mL of concentrated H2S04 and 3 mL of concentrated HN03 and dilute to 100 mL. This solution contains 1000 pg/mL of mercury. 6.5 Mercury Standard, Working (0.1 jig/mL)--Make suc cessive dilutions of the stock mercury solution to obtain a working standard containing 0.1 mg/L (0.1 jig/mL), main taining a concentration of 5 % H2S04 and 3 % HN03 by volume, in the diluted solutions. The working mercury standard and the dilutions of the stock mercury solution should be prepared fresh each day that it is used. 6.6 Nitric Acid (sp gr 1.42)--Concentrated nitric acid (HN03). 6.7 Nitrogen. 6.8 Potassium Permanganate Solution (0.1 N)--Dissolve 15.8 g of KMn04 in water and dilute to 1 L. 6.9 Stannous Chloride Solution (100 g/L)--Dissolve 25 g of tin (II) chloride (SnCl2) by adding it to 60 mL of concentrated HC1 (sp gr 1.19) and warming on a hotplate. When all of the SnCl2 has dissolved, transfer to a 250-mL volumetric flask and dilute to volume with water. Mix well. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." This solutioa should be prepared fresh each week that it is used. 6.10 Sulfuric Acid (sp gr 1.84)--Concentrated sulfuric arid (H2S04). 6.11 Sulfuric Acid (1+9)--Carefully mix 1 volume pf H2S04 (sp gr 1.84) into 9 volumes of water. 7. Hazards - ! [ i \ s' 8.6 record recorc tube f bottle the at the m 7.1 Concentrated nitric and sulfuric acids are corrosive [ and may cause severe bums of the skin or eyes. The vapor I from concentrated nitric arid is irritating to mucous mem- \ Noi avoid i an abs solutic branes. Use care in handling these acidic substances. Refer to : soluric suppliers' Material Safety Data Sheet. 7.2 Mercury and its compounds are harmful and accumulate in the aquatic environment. Mixtures containing mercury compounds should not be flushed down a drain, but \ 8.7 versu the n disposed of as hazardous waste. 5 7.3 Use only a rubber bulb aspirator for pipetting liquids, s 9. Pi 9.1 8. Calibration and Standardization neou 8.1 Assemble the various components, as illustrated in Fig. 1 if an atomic absorption spectrophotometer is used, or prepare the instrument for operation if a commercial mer cury analyzer is being used. N' 2--Be sure that all glassware has been thoroughly cleanecfMd rinsed with reagent water prior to use. . ; least diffe of t decc (140 9. rerrr 8.2 Operational instructions for atomic absorption ! tiall; spectrophotometers and commercial mercury analyzers vary j heat with different models. Consult the manufacturer's literature j for establishing optimum conditions for the specific instiu- j ment used. j 9.1 and into 8.3 With the apparatus, empty, stabilize the recorder base line while maintaining a flowrate of 250 mL of nitrogen per j minute. ! 8.4 Transfer 0, 5, 10, 15, and 20-mL aliquots of the i working mercury standard (containing 0 to 2 pg of mercury) Nt strate subst labor glass to a series of 250-mL gas washing bottles. Add enough water a un to each bottle to make a total volume of 100 mL. Add 5 mL of H2S04 and 3 mL of HNQ3 to each bottle and mix film film thoroughly. Make dropwise additions of 0.1 N KMnOj 9. solution to each bottle in turn until" a pink color persists for | con' at least 30 s (1 mL is usually sufficient). Add exactly 1 mL of | usir NH2OH-HCI solution dropwise to each bottle and swirl and 540 DUPO 502 97721 that it is sulfuric lume of :orrosive te vapor ts memRefer to iccumung merain, but liquids. rated in tsed, or il mer- ned and irption ers vary terature ; instru- ier base >gen per of the tercury) >h water Id 5 mL nd mix KMn04 sists for 1 mL of id swirl 1 D 3624 until the pink color is discharged. 8.5 Add 10 mL of SnCl2 solution to the bottle containing no added working mercury standard. Immediately insert the fritted glass inlet tube, making sure that the stopper provides a good seal. Adjust the nitrogen flow rate to a previously determined optimum setting (see Note 3) and take a reading. A blank value greater than 5 % of full scale indicates either reagent or apparatus contamination. When the recorder, meter, or other readout device reaches a maximum value, it should be immediately zeroed. Repeat this blank determina tion until a steady, repeatable zero value is obtained at the maximum response. N' 3--Optimum nitrogen flow rate may be determined by ana lyzing 1-ug quantities of mercury (10 mL of working mercury standard diluted to 100 mL) by this procedure, varyingthe flow rateto determine the optimum mercury signal and time required for analysis. Then use this optimum flow rate for all analyses, unless a change is made in the volume or geometry of the apparatus. 8.6 Similarly treat each standard solution made up in 8.4, recording the maximum peak height for each. When the recorder pen begins dropping, remove the fritted glass inlet tube from the gas washing bottle and insert it into another bottle containing only water. Continue nitrogen flow until the absorbance reaches zero, when the apparatus is ready for the next solution. N !' 4--Because mercury vapor is very toxic, take precautions to avoid its inhalation. Bubble the exhaust from the absorption cell through an absorbing solution consisting of equal volumes of 0.1 N KMn04 solution and 10 % H2S04 (see Fig. 1). Do not discharge the absorbing solution into a sewer system. 8.7 Construct a standard curve by plotting peak heights versus micrograms of mercury. Peak heights used should be the mean of duplicate determinations on each solution. 9. Procedure 9.1 If the sample is a liquid coating, mix it until homoge neous, preferably on a mechanical paint shaker. Prepare at least two replicate specimens by weighing to 0.1 mg by difference from a dropping bottle or syringe, 100 to 200 mg of the mixed paint into the PTFE insert of the acid decomposition vessel. Place the insert in an oven set at 60"C (140F) for 1 h to remove all volatiles. 9.1.1 Caution--If the solvent present in a sample is not removed prior to the digestion step as recommended, poten tially dangerous pressures may result when the vessel is heated at 140C. 9.2 If the sample consists of dried film, coarsely grind it and weigh 50 to 100 mg by difference from a weighing bottle into the digestion vessel. N"#' 5--Recover dried paint films from previously coated sub strates (being careful not to remove any underlying material from the substrate) or prepare in the laboratory from liquid samples. For the laboratory preparation, flow some ofthe well-mixed sample onto a clean glass plate. The use of a paint draw-down bar is recommended to obtain a uniform wet film thickness not exceeding 2 mils (50 pm). Allow the film to dry in an oven at 60C for a minimum of 1 h. Scrape the dried film off the glass plate, preferably with a single-edge razor blade. 9.3 Pipet 5 mL of concentrated H2S04 and 3 mL of concentrated HNOs into the decomposition vessel insert, using a fume hood for the operation. Seal the vessel tightly and place in the circulating oven at 140'C for 1V2 h. Remove the vessel from the oven and allow it to cool slowly to room temperature. NOTE 6--Do not assist cooling by putting the vessel in a refrigerator or freezer, or by submerging it in a cooling liquid; otherwise mercury losses may occur due to leakage of pressurized gases resulting from uneven contraction of the bomb parts and PTFE seal. N"#' 7--Analysis of the digested specimen (9.4 to 9.7) should be completed within 1 h after the digestion step. 9.4 When completely cooled, carefully unseal the vessel in a fume hood, add approximately 5 mL of cold water and swirl gently. Quantitatively transfer the contents to a 100-mL beaker, using several small quantities of water. Dilute to a volume of 30 to 40 mL and filter through filter paper directly into a 100-mL volumetric flask. Wash the residue on the filter paper several times with small volumes of water. Dilute to volume with water and mix thoroughly. 9.5 Transfer an aliquot of each digested specimen con taining not over 2 jxg of mercury to a 250-mL gas washing bottle. Add enough water to make a total volume of 100 mL. To each bottle, add 5 mL of concentrated H2S04 and 3 mL of concentrated HN03 and mix thoroughly. N$%' 8--If large aliquots are taken for analysis, reduce the amount of added H2S04 and HN03 proportionately to compensate for the amounts present in the digested solutions. 9.6 Proceed with the addition of KMn04, NH2OH>HCl, and SnCl2 solutions as described in 8.4 and 8.5. Record the maximum peak height for each solution. 9.7 If the response obtained is above or below the response obtained for the standards (8.7), repeat 9.5 and 9.6 using an appropriate aliquot size. Determine the concentra tion of mercury present in microgram per millilitre from the calibration curve. 10. Calculation 10.1 Calculate the mean concentration of mercury in the sample as follows: mercury in sample, ppm (mg/kg) = (100 x C)/(F x 5) where: C = concentration of mercury in aliquot used, pg/mL, F = dilution factor from 9.5 (aliquot volume used), and S -- grams of sample. 11. Report 11.1 Report the mercury content in the material being tested and whether the analysis was conducted on a liquid coating or a dried film. 12. Precision and Bias5 12.1 Precision--The precision estimates are based on an interlaboratory study in which seven different laboratories analyzed in duplicate, on two different days, four samples of water-reducible paints and four samples of solvent-reducible paints containing from 1 to 1000 ppm mercury. The within laboratory coefficient of variation was found to be 6.4 % relative at 42 degrees of freedom, and the between-laboratory coefficient of variation 10% relative at 36 degrees of freedom. Based on these coefficients, the following criteria 5 Supporting data are available from ASTM Headquarters. Request RR: D01-1006. 541 DU P050297722 >3624 should be used for judging the acceptability of results at the 95 % confidence level: 12.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator on different days, should be considered suspect if they differ by more than 18 % relative. 12.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories, should be considered suspect if they differ ( , more than 30 % relative. ^ 12.2 Bias--The true value for the amount of mercujv present in a coating should be between 79 and 121 % ofy^ experimental value. 13. Keywords 13.1 AAS, mercury; low concentration of mercury j5 paints Des The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapprovedor withdrawn. Your comments are invited either lor revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feetthat your comments have not received a fair hearing you should make your views known to the ASTM Committee onStandards, 1916 Race St., Philadelphia, PA 19103. j. Scope ' i.i Thi; products,.. of analyti' ettce and potential F 1.2 Va ' and regu presence i protectiv within tf 1.3 A one tha ingestioi Hazards 1.4 1 cttions, address the res. ; approp applicc 2. Ref 2.1 D4' D1 C i D D D D D D r 'A. I Re! DO pul 542 DUP050297723 Designation: D 3630 - 89 Standard Guide for Determining Constituents Classified as Hazardous Contained in Protective Coatings1 This standard is issued under the fixed designation D 3630; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1, Scope 1.1 This guide applies to liquid protective coatings, related products, and their dried films. It is a guide for the selection of analytical procedures for the determination of the pres ence and quantity of selected materials that may present potential physiological hazards. 1.2 Various levels of government have established laws and regulations that limit the quantity or prohibit the presence of certain materials classified as hazardous in protective coatings. Materials subject to such regulations are within the scope of this guide. 1.3 A hazardous material within the scope of this guide is one that exhibits harmful physiological effects through ingestion, inhalation, absorption, or skin or eye contact. Hazards associated with combustion are not within its scope. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 49 Methods of Chemical Analysis of Red Lead2 D126 Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium Oxide Green2 D215 Methods of Chemical Analysis of White Linseed Oil Paints3 D283 Methods of Chemical Analysis of Cuprous Oxide and Copper Pigments2 D 444 Test Methods for Chemical Analysis of Zinc Yellow Pigment (Zinc Chromate Yellow)2 D 564 Test Methods for Liquid Paint Driers4 D715 Test Methods for Analysis of Barium Sulfate Pigment2 D1301 Test Methods for Chemical Analysis of White Lead Pigments2 D1844 Test Methods for Chemical Analysis of Basic Lead Silicochromate2 1 This guide is under the jurisdiction of ASTM Committee D*1 on Paint and. Related Coatings and Materials and is the direct responsibility of Subcommittee 001.22 on Health and Safety. Current edition approved Oct. 27, 1989. Published December 1989. Originally Published as D 3630-77. Last previous edition D 3630-77 (198I)l. 2 Annual Book ofASTMStandards, Vol 06.02. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards* Vol 06.03. D1845 Test Methods for Chemical Analysis of Strontium Chromate Pigment2 D 2348 Test Method for Arsenic in Paint3 D 2349 Method of Qualitative Determination of Nature of Thinner in Solvent-Reducible Paints3 D2350 Test Method for Antimony Oxide in White Pigment Separated From Solvent-Reducible Paints2 D2371 Test Method for Pigment Content of Solvent- Reducible Paints3 D 2372 Method of Separation of Vehicle From Solvent- Reducible Paints3 D 2374 Test Method for Lead in Paint Driers by EDTA Method4 D2621 Test Method for Infrared Identification of Vehicle Solids From Solvent-Reducible Paints3 D 2698 Method for Determination of the Pigment Content of Solvent-Reducible Paints by High-Speed Centri fuging3 D2742 Methods for Chemical Analysis of Tribasic Lead Phosphosilicate2 D 3257 Test Methods for Aromatics in Mineral Spirits by Gas Chromatography4 D 3271 Practice for Direct Injection of Solvent-Reducible Paints Into a Gas Chromatograph for Solvent Analysis3 D 3272 Practice for Vacuum Distillation of Solvents From Solvent-Reducible Paints For Analysis3 D 3280 Methods for Analysis of White Zinc Pigments2 D 3329 Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography4 D3335 Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy3 D3432 Test Method for Free Toluene Diisocyanates in Urethane Prepolymers and Coating Solutions by Gas Chromatography2 D3618 Test Method for Detection of Lead in Paint and Dried Paint Films3 D 3624 Test Method for Low Concentrations of Mercury in Paint by Atomic Absorption Spectroscopy3 D 3717 Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy3 D3718 Test Method for Low Concentrations of Chro mium in Paint by Atomic Absorption Spectroscopy3 E 202 Test Methods for Analysis of Ethylene Glycols and Propylene Glycols5 E 260 Practice for Packed Column Gas Chromatography6 3 Annual Book ofASTM Standards, Vol 15.05. 6 Annual Book ofASTM Standards. Vol 14.01. 543 DUP050297724 D.3630 2.2 ANSI Standard: Z66.1 Specification for Paints and Coatings Accessible to Children to Minimize Dry Film Toxicity7 2.3 Federal Standards:* U.S. Federal Test Method Standard No. 141: 4021.1 Pigment Content (Ordinary Centrifuge) 4032 Vehicle Isolation (Super Centrifuge) 7041 Analysis of Basic Carbonate White Lead Pigment 7051 Analysis of Basic Sulfate White Lead Pigment 7071 Red Lead Pigments 7106 Analysis of Antimony Oxide Pigment 7111 Analysis of Chrome Green Pigment 7131 Analysis of Chrome Yellow and Chrome Orange Pigments 7135 Analysis of Cadmium Pigment 7231 Metal Content of Driers 7271 Analysis of Pigments Extracted from Chrome Yellow and Chrome Orange Paints 7281 Analysis of Pigment Extracted from Chrome Green Paints 2.4 Canadian Standards Association Standards:9 CAN2-1.500 Method of Test for Toxic Trace Elements in Protective Coatings: l-GP-500.1 Determination of Lead in Low Concentra tion l-GP-500.2 Determination of Teachable Cadmium in Low Concentration l-GP-500.3 Determination of Leachable Barium in Low Concentration l-GP-500.4 Determination of Leachable Antimony in Low Concentration l-GP-500.5 Determination of Leachable Selenium in Low Concentration l-GP-500.6 Determination of Leachable Mercury in Low Concentration 3. Summary of Guide 3.1 This guide covers each material separately, discussing the methods available, the advantages and drawbacks of each, including the range, the equipment needed, and when information is available, the precision. Methods discussed are: . 3.1.1 ASTM methods adopted by Committee D-l, 3.1.2 Other ASTM methods believed to be applicable to paint and related products, 3.1.3 Methods adopted as standard by other scientific and technical or governmental organizations, and 3.1.4 Widely used methods reported in .the literature. 4. Significance and Use 4.1 Protective coatings and related products containing materials classified as hazardous may be regulated or con trolled in various ways as follows: 4.1.1 Precautionary Labeling Required: 7 Available from American National Standards institute, 11 W. 42nd St.. 13th Floor, New York, NY 10036. '8 Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094. 9 Available from Canadian Standards Association, 17S Rexdale Blvd., Rexdaie, Ontario, Canada M9W 1R3. 4.1.1.1 Under the U.S. Federal Hazardous Substances Act and corresponding state laws, "consumer" paint products must carry precautionary labeling as specified in the laws, or implementing regulations, or both. N&'' 1--Under the Federal Hazardous Substances Act lead, ethylene and diethylene glycol, petroleum distillates, and turpentine are classed as hazardous through ingestion. Methyl alcohol, benzene, xylene, and toluene are classed as hazardous through ingestion and inhalation! Ethylene diamine, diethylene triamine, and diglycidyl ethers are classed as strong sensitizers. 4.1.1.2 In certain states, coatings and related materials packaged and sold for industrial application are subject to precautionary labeling laws and regulations. 4.1.2 Use Prohibited in Certain Areas: 4.1.2.1 Under the U.S. Federal Hazardous Substances Act and the Lead Paint Poisoning Prevention Act, and the laws of certain states and municipalities, coatings and related products containing more than a specified quantity of lead are banned for use in and around a household or other areas where children might be exposed. 4.1.2.2 Under certain local ordinances, coatings and re lated products containing more than a specified quantity of "other toxic heavy metals" are also subject to control. N&'' 2--The amount of lead, antimony, arsenic, cadmium, mer- cury, selenium, and soluble barium that may be present in coatings for use on children's furniture and toys and areas that might be chewed by children is restricted under ANSI Standard Z66.1 and under various U.S. municipal ordinances. 4.1.3 Subject to Approvalfor Certain Uses: 4.1.3.1 The U.S. Food and Drug Administration permits only approved ingredients to be used in coatings for food and beverage containers or processing equipment that comes into contact with the product. 4.1.3.2 The U.S. Department ofAgriculture authorizes for use on structural surfaces in federally inspected meat and' poultry processing plants only coatings accepted as nonhazardous. 4.1.3.3 The U.S. Environmental Protection Agency regu lations control the distribution of paints that claim special fungicidal or pesticidal characteristics, and the use in shipbottom paints of materials that haVe the potential for harming the aquatic environment. N&'' 3--Cuprous oxide, bisftributyltin oxide), arsenic, and mercury are classed as hazardous materials by the U.S. Environmental Protection Agency when used in antifouling paints. 4.1.4 Environmental Controls During Use and Corrective Measures in the.Event ofAccidents or Misuse Required: 4.1.4.1 Under U.S. Occupational Safety and Health Act regulations, airborne concentrations of certain vapors, fumes, and dusts are limited in the work-place atmosphere. Coatings, when applied, may emit solvent vapors that are subject to these limits. 4.1.4.2 Under Occupational Safety and Health Act regu lations, skin or eye contact with liquid paint containing specified potentially hazardous materials must be avoided and protective apparel may be required. Tn the event of hazardous skin or eye contact, corrective action to amelio rate physiological injury is prescribed. N*+' 4--Over 400 materials have been classified by the Occupa tional Safety and Health Administration as being potentially hazardous. 544 Of this m compone: 4.1.4.. Air Act emissioi applicat 5. Pigir 5.1 1 separati be anal) method absorpt: speed.a 5.2 S the firs method 5.2.1 laborati where ; ment ii 5.2.2 fuge th vehicle 5.2.3 develoj conten separat residua N()' of pigmi particle 5.3 centrif Metho are list lacque but ha 4021.! 6. Sol 6.1 dure t of pai 6.2 injecti Prior: 7. He 7.1 pigme ance \ 7.2 7.2. excep which DUP050297725 # 0 3630 5 Act iucts ;s, or lead, ie are jiene, ation. assed -`rials A to ; Act laws ated lead ureas 1 re:y of meris for ;d by nous mits and into 3 for and as igu cial ipfor ary ion (eve Act ors, ere. are cu ring ded : of :lio- upaous. : ; Qfthis number approximately 80 may be found in varying amounts as ; ^jnponents of coatings and related products.10 4.1.4.3 To achieve air quality standards under the Clean ;jr Act, regulations of various states and regions control eInissions of volatile organic compounds resulting from the application of surface coatings. j, pigment, Vehicle Separations (Centrifugal) 5.1 The methods listed in this section cover centrifugal separation of pigment from vehicle. The pigment may then be analyzed as described in subsequent sections. More recent methods utilizing analysis of the whole paint by atomic absorption spectroscopy may be preferred due to greater speed and accuracy. 5.2 Separation of the vehicle from the pigment is generally (be first step in coatings analysis. There are three ASTM methods covering the use of centrifuges: 5.2.1 Test Method D 2371 describes the use of the normal laboratory centrifuge that develops 2000 g. It should be used where a quantitative determination of the amount of pig ment in the coating is required. 5.2.2 Method D 2372 covers use of a high-speed centri fuge that develops 10 000 g and is used when analysis of the vehicle is of main interest. 5.2.3 Method D 2698 covers use of a centrifuge that develops at least 32 000 g. Determination of the pigment content is the main objective of the method although the separated pigment may be solvent-extracted to remove residual vehicle. N,-' 5--Centrifuge methods do not generally give good separations of pigments that bleed (partially dissolve) or have low densities and fine particle sizes (such as carbon black). 5.3 U.S. Federal Test Method Standard 141 contains two centrifuge methods. Federal Method 4021.1 is similar to Test Method D 2371 except that additional extraction mixtures are listed for difficult pigments and for cellulosic and vinyl lacquers. Federal Method 4032 is similar to Method D 2698 but has the same extraction solvents as in Federal Method 4021.1. 6. Solvent Separation 6.1 Practice D 3272 covers a vacuum distillation proce dure that separates the solvents from the nonvolatile portion of paints so they may be analyzed. 6.2 Practice D3271 covers analysis of the solvents by injection of the liquid coating into a gas chromatograph. Prior separation is not required. ANALYTICAL METHODS 7. Heavy Metals Analysis, ASTM Methods 7.1 Methods for the analysis of pigments apply to dry pigment or to pigment separated from the vehicle in accord ance with Section 5. 7.2 Lead: 7.2.1 Pigment Analysis--In all the following methods except for Methods D2742, the concentration range for which the method is applicable is not given. 10Occupational Safety and Health Reporter, Section 1910.1000 Table Z.l. 7.2.1.1 Methods D49 cover procedures for the chemical analysis of dry red lead having the approximate formula Pb304 (probably Pb02-2Pb0). Total lead is determined gravimetrically as lead sulfate. 7.2.1.2 Test Methods D 126--Total lead is determined gravimetrically as lead sulfate. The comparable Fed. Test Methods Std. 141 methods are 7271 and 7281. 7.2.1.3 Methods D215--Two methods are described for the gravimetric determination of total lead, one as the sulfate and the other as the chromate. The choice of method may be dictated by potential interferences discussed in the text. 7.2.1.4 Test Methods D 1301 cover procedures for the chemical analysis of basic carbonate white lead and basic sulfate white lead. Total lead is determined gravimetrically as lead chromate. The comparable Fed. Test Method Std. 141 method is 7041. 7.2.1.5 Test Methods D 1844--Total lead is determined gravimetrically as lead chromate. 7.2.1.6 Methods D 2742--Silicon is removed by filtration and total lead determined gravimetrically as lead sulfate. The methods are designed for the analysis of essentially pure pigment. 7.2.1.7 Methods D 3280 cover procedures for the analysis of white zinc pigments, including leaded zinc oxide. Total lead is determined gravimetrically as lead sulfate. 7.2.2 Analysis ofLiquid Material or Dried Film: 7.2.2.1 Test Methods D564 cover the determination of percent lead in liquid driers (see Section 9). Total lead is determined gravimetrically as lead sulfate. The comparable Fed. Test Method Std. No. 141 method is 7231. 72.2.2 Test Method D 2374 covers a titrimetric determi nation of lead in paint driers that can be dissolved in a suitable solvent and utilizes excess EDTA (ethylene diamine tetraacetic acid) to react with lead and cupric sulfate to back titrate. The drier is dissolved in glacial acetic acid, diluted with isopropyl alcohol and water, and treated with an excess of standard EDTA solution. The excess is titrated with standard cupric sulfate solution using an indicator. The method includes a precision statement but the applicable concentration range is not given. 7.2.2.3 Test Method D 3335 covers the determination of lead contents between 0.01 and 5 % present in the solids of liquid coatings or in dried films. A specimen of liquid paint or dried film is prepared for analysis by dry ashing. The lead content of an acid extract of the ash is determined by atomic absorption spectroscopy. The precision statement is based on a relative scale. 7.2.2.4 Test Method D 3618 is intended as a screening test to determine if a sample of paint solids contains more than 0.5 % lead. The test will barely detect the presence of 0.4 % and will give a definite test at the 0.5 % level. The specimen is dry ashed and extracted. Lead present is oxidized to lead peroxide and, spotted with "tetrabase" to develop a blue coloration. Higher or lower concentrations may be detected by this test method by making appropriate changes in the specimen size and reagent quantities. 7.3 Chromium: 7.3.1 Pigment Analysis: 7.3-. 1.1 Test Methods D 126--In these test methods the chromium content of pigments is only calculated as Cr203 for chromium oxide green. For chrome oranges, yellows, and 545 DUP0502 97726 D 3630 greens the chromium is calculated as lead'chromate. 7.3.1.2 Test Methods D444 cover procedures for the chemical analysis of the pigment known commercially as "zinc yellow" or "zinc chromate yellow." Total chromium in the pigment is determined by titration using either the dichromate method or the thiosulfate method and calculated as Cr03. 7.3.1.3 Test Methods D 1844--Total chromium in the pigment is determined as chromium trioxide by titration using the thiosulfate method. 7.3.1.4 Test Methods D 1845--Total chromium in the pigment is determined as chromium trioxide by titration using the thiosulfate method. 7.3.2 Analysis ofLiquid Paint or Dried Film: 7.3.2.1 Test Method D 3718 covers the determination of chromium or chromium compounds (including chromium oxide) when present in the solids of liquid coatings or in dried films in the concentration range from 0.005 to 1.0 % (50 to 10 000 ppm) expressed as chromium. A specimen of liquid paint or dried film is prepared for analysis by dry ashing. A weighed quantity of the ash is digested with potassium permanganate and sulfuric acid. Chromium is determined on the filtered digestion mixture by atomic absorption spectroscopy. 7.4 Barium: 7.4.1 Pigment Analysis: 7.4.1.1 Methods D215--Soluble barium is determined gravimetrically as the sulfate. 7.4.1.2 Test Methods D 715--Applicability to mixed pig ments when barium is a minor component is not indicated. 7.4.1.3 Methods D 3280 cover procedures for the analysis of white zinc pigments. Determination of total barium sulfate content is described in Section 20 of Methods D 3280. 7.4.2 Analysis of Liquid Paint or Dried Film--Current legislation restricts the quantity of "soluble" barium in coatings used in areas accessible to children, but the condi tions of solubility are not usually defined. There is no ASTM method for soluble barium; see Section 10. 7.5 Mercury: 7.5.1 Analysis of Liquid Paint or Dried Film--Test Method D 3624 covers the determination of mercury con tents between 10 and 1000 ppm in liquid coatings and dried films. The specimen of whole paint, paint vehicle, or dried film is digested using sulfuric and nitric adds, and the concentration of mercury determined using cold-vapor atomic absorption. 7.6 Arsenic: 7.6.1 Analysis of Liquid Paint or Dried Film--Test Method D 2348 covers the determination of less than 0.5 % arsenic in liquid coatings or dried films. Whole paint or dried film is digested in nitric and sulfuric add. Sodium chloride is added and the arsenic trichloride distilled. Total arsenic is determined by titration with potassium bromate. 7.7 Antimony: 7.7.1 Pigment Analysis: Test Method D 2350--Total an timony is calculated from the antimony oxide content determined by titration with potassium permanganate. The concentration range for which the method is applicable is not given. The comparable Federal Method is 7106. 7.7.2 Analysis of Liquid Paint or Dried Film--Test Method D3717 covers the determination of antim contents between 50 and 200 ppm present in the solids^ liquid coatings in dried films. The specimen of liquid or dried film is prepared for analysis by dry ashing at 5oor followed by refluxing with hydrochloric acid and stannci chloride. The antimony content of the acid extract ^ determined by atomic absorption spectroscopy. 18 7.8 Cadmium: 7.8.1 Analysis of Whole Paint or Dried FUm--.'x^ Method D3335 covers the determination of cadmium contents between 50 and 150 ppm present in the solids of liquid coatings or in dried films. The sample of liquid paint or dried film is prepared for analysis by dry ashing. The content of cadmium is determined by atomic absorption . spectroscopy. 8. Other Regulated Metallic Components 8.1 Copper: 8.1.1 Pigment Analysis--Methods for the. analysis of the pigment portion of the coating after separation. 8.1.2 Methods D283 cover analysis for total copper in copper-based pigments. 10 <0 qua1 coat Hl terb by pro- 12- 1 be co' sta He chsai 9. U.S. Federal Test Method Standard No. 141 j 9.1 Lead: 4 9.1.1 Method 7041 is comparable to Test Methods^ D1301. - 9.1.2 Method 7051 is comparable to Test Methods*? ' D1301. 9.1.3 Method 7071.1 is for the quantitative measure of . f red lead in paint pigments. ,;j 9.1.4 Method 7111 is comparable to Test Methods D 126:, s 9.1.5 Method 7131 is comparable to Test Methods D 126. I f 9.1.6 Method 7231 is comparable to Test Methods D 564,- ; * 9.1.7 Method 7271 is comparable to Test Methods D126., 9.1.8 Method 7281 is comparable to Test Methods D 126. ` : 9.2 Antimony: f: 9.2.1 Method 7106 is comparable to Test Method-- < D 2350. Jj 9.3 Cadmium: ; 9.3.1 Method 7135. ,4| S so a cc ai ft 10. Other Analytical Methods for Materials Gassed as;. Hazardous Within the Scope of This Practice 10.1 National Standard of Canada CAN2-1.5Q0.describes test methods for determining toxic elements in low conceit-: trations in protective coatings, employing wet chemical andv atomic absorption and visible-ultraviolet spectrophotometric techniques. Determination of leachable elements are made f \ on a dilute hydrochloric acid extract of the dried film that * has first been ground to a specific fineness. >> 5 10.1.1 I-GP-500.1 is used for determining total lead in liquid and applied coatings by atomic absorption spectros-rs copy. .-si 10.1.2 l-GP-500.2 is used for determining soluble cad-1 | mium in applied coatings! by atomic absorption spectres- f | copy. ..... 10.1.3 l-GP-500.3 js used for determining soluble barium-. J in applied coatings by atomic absorption spectroscopy. 10.1.4 l-GP-500.4 is used for determining soluble anti mony in applied coatings by visible-ultraviolet spectroscopy. 546 DUP0502 97727 mony ids of paint 500'C nnous act is -Test mium ids of paint The ption of the aer in thods 'thods ire of > 126. ) 126. ) 564. ) 126. ) 126. ethod D 3630 10.1.5 l-GP-500.5 is used for determining soluble sele nium in applied coatings by visible-ultraviolet spectroscopy. 10.1.6 l-GP-500.6 is used for the detection of, and the quantitative determination of, soluble mercury in applied coatings by visible-ultraviolet spectroscopy. 11. Nonvolatile Vehicle Components, ASTM Methods 11.1 Test Method D2621 covers the qualitative charac terization or identification of separated paint vehicle solids by infrared spectroscopy within the limitations of this procedure. j2. Volatile Components 12.1 The volatile components of protective coatings must be identified to determine compliance with regulations covering labeling, work place concentrations, and air quality standards. 12.2 Gas chromatography is widely used for this purpose. However, owing to the empirical nature of the technique, chemical or instrumental confirmatory tests may be neces sary as supplementary procedures. 12.3 Identification of the components of an unknown solvent blend would in many cases be expedited by means of a combination ofgas chromatography and infrared spectros copy or mass spectrometry. 12.4 Interconnected chromatographic, infrared analyzers are available that separate multicomponent mixtures into their pure components for infrared analysis. 12.5 Analysis of the volatile component of whole paint has been covered in Section 6. 12.6 The following ASTM methods cover the analysis of some of the volatile components of protective coatings currently subject to regulation as potentially hazardous materials: 12.6.1 Method D2349 covers the determination of the nature of thinner in solvent-reducible house paints con taining only hydrocarbon solvents. 12.6.2 Test Method D 3432 covers low molecular weight urethane products containing (a) 0.1 to 1.0 % and (b) 1.0 to 10 % of free toluene diisocyanate (TDI) content. 12.6.3 Test Methods D 3257 cover the determination of ethylbenzene and total eight-carbon (Cg) and heavier aro matics in the concentration range from 0.1 to 30% in mineral spirits having a distillation range from 300 to 410F (150 to 210C). Oxygenated compounds, if present, may interfere and cause erroneous results. 12.6.4 Method D 3329 covers the determination of the purity of methyl isobutyl ketone by gas chromatography. 12.6.5 Test Methods E202--See Sections 26 to 35 (Gas Chromatographic Techniques). 12.6.6 Practice E 260. 13. Keywords 13.1 antimony; aromatics; barium; cadmium; Canadian methods; chromium; copper; government regulations; haz ardous substances; heavy metals; lead; mercury; pigments; selenium; solvents; zinc The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of (he responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. d as ribes ncenil and netric made l that ad in ctros- : cadctros- arium antiicopy. DUP050297728 Designation: D 3717 - 85a (Reapproved 1991)c1 Standard Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy1 This standard is issued under the fixed designation D 3717; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (' ) indicates an editorial change since the last revision or reapproval. " N./' --Keywords were added editorially in July 1991. ( so! 1.' Itv 1. Scope 1.1 This test method covers the determination of the content of antimony in the range between 50 and 200 ppm (mg/kg) present in the solids of liquid coatings or in dried films obtained from previously coated substrates. There is no reason to believe that higher levels could not be determined by this test method, provided that appropriate dilutions and adjustments in specimen size and reagent quantities are made. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. Specific hazard statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D1193 Specification for Reagent Water2 D 2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings3 an atomizer and either a single- or three-slot burner, pressure regulating and metering devices for air and acety lene; an antimony source lamp with a regulated constant current supply; a monochromator and associated optics; a photosensitive detector connected to an electronic amplifier, and a readout device. 5.2 Muffle Furnace, maintained at 500 10C. 5.3 Oven, maintained at 105 2C. 5.4 Hot-Plate, with variable surface temperature control over the range from 70 to 200C. 5.5 Reflux Condenser, water-cooled, and fitted with a standard-taper joint. 5.6 Erlenmeyer Flask, 125-mL, with standard-taper joint to fit condenser. 5.7 Volumetric Flasks, 100 and 1000-mL. 5.8 Dropping Bottles, lA or Vi-oz (8 or 15-mL) capacity. 5.9 Glass or Disposable Syringes, 10-mL capacity. 5.10 Pipets, 1, 5, 10, and 15-mL capacity. 5.11 Filter Paper, ashless, medium or slow filtering, 5.12 Paint Shaker. 5.13 Paint Draw-Down Bar. 3. Summary of Test Method 3.1 The sample of liquid coating or dried film is prepared for analysis by dry ashing at 500C, followed by refluxing with hydrochloric acid and stannous chloride. The antimony content of the acid extract is determined by atomic absorp tion spectroscopy. 4. Significance and Use 4.1 The permissible level of heavy metals in certain coatfngs is specified by govemmenfal regulatory agencies. This test method provides a fully documented procedure for determining low concentrations ofantimony present in both water- and solvent-reducible coatings to determine compli ance. 5. Apparatus 5.1 Atomic Absorption Spectrophotometer, consisting of ' This test method is under the jurisdiction of ASTM Committee D-i on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO!.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 31 and Nov. 29, 1985. Published January 1986. Originally published as D 3717 - 78. Last previous edition D 3717 - 84. 2 Annua/ Boole ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vo106.0!. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.4 Other ] grades may be used, provided it is first ascertained that the j reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent grade; water conforming to Type II of Specification D 1193. 6.3 Antimony Standard Stock Solution (0.1 mg/mL)-- Dissolve 0.1000 g of antimony metal in 40 mL of sulfuric acid (H2S04, sp gr 1.84) by heating. Cool, carefully transfer \ quantitatively to a 1-L volumetric flask already approxi mately half full with water, allow to cool to room tempera ture, and dilute to 1 L. 4 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostiand Co., Inc., New York, NY, and the "United States Pharmacopeia." 548 8 DUP0502 97729 D3717 6.4 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro chloric acid (HC1). 6.5 Stannous Chloride Solution (400 g/L in HC1)--Dis solve 40 g of tin (II) chloride (SnCl2) in 50 mL of HC1 (sp gr 1.19). Transfer to a 100-mL volumetric flask and fill to the ,jiark with concentrated HC1. 7. Hazards 7.1 Use care in handling concentrated HCI because it is corrosive and may cause bums to the skin and eyes and its vapor is irritating to mucous membranes. Refer to suppliers' Material Safety Data Sheet. 7.2 Use only a rubber bulb aspirator for pipetting liquids. g. Calibration and Standardization 8.1 Prepare 100-mL quantities of at least four standard solutions bracketing the expected antimony concentration in the sample to be tested. To suitable aliquots of the 0.1 mg/mL standard antimony solution, add 40 mL of concen trated HCI and 8 drops of SnCl2 solution. Dilute to 100 mL with water. Prepare a blank solution by diluting 40 mL of concentrated HCI and 8 drops of SnG2 solution to 100 mL with water. 8.2 Operational instructions for atomic absorption spectrophotometers vary with different models. Consult the manufacturer's literature for establishing optimum condi tions for the specific instrument used. 8.3 Turn the instrument on and set the wavelength to the 217.6-nm antimony line. Apply the recommended current to the antimony source lamp. Allow the instrument to warm up for about 15 min and set the slit width. Adjust the air and acetylene pressures and ignite the burner in accordance with instructions. 8.4 Aspirate water to rinse the atomizer chamber. Aspi rate a standard solution and make any necessary readjust ment in instrument parameters to obtain maximum absorp tion. 8.5 Aspirate the blank solution. When the recorder, meter, or other readout device reaches a constant value, it should be immediately zeroed. Repeat this blank determina tion until a steady, repeatable zero value is obtained at the maximum response. 8.6 Aspirate each of the appropriate standard solutions in ascending antimony concentrations and record the corre sponding instrument readings. Aspirate water between each standard N01' 1--A deuterium background corrector, if available, should be used to correct for background absorption. If not available, it is necessary to reaspirate each standard solution and measure the back ground at a nearby nonabsorbing region of the spectrum. N23' 2--Because of the high concentration and corrosive nature of the acids used for the analysis, it is essential that the burner assembly be disassembled and thoroughly cleaned out immediately after the analyses are completed. Consult the instrument manual for cleaning instructions. 8.7 Construct a calibration curve on linear graph paper by plotting the absorbance (corrected for background) versus concentration (micrograms per millilitre) for each standard solution. 9. Procedure 9.1 If the sample is a liquid coating, mix it until homoge neous, preferably on a mechanical paint shaker. Determine the nonvolatile content in accordance with Guide D 2832. 9.2 Prepare at least two replicate samples by weighing by difference from a dropping bottle or syringe, 5 to 10 g of the mixed liquid coating, or by directly weighing approximately 2 to 6 g of dried film, into 125-mL Erlenmeyer flasks. Weigh to the nearest 0.1 mg. N45' 3--The specimen size called for will have a concentration of approximately 4 to 12 gg/mL antimony in the final diluted solution for paints containing approximately 200 ppm (mg/kg) antimony based on the nonvolatile content, and 1 to 3 pg/mL for paints containing approximately 50 ppm antimony, based on the nonvolatile content. N01' 4--Recover dried paint films from previously coated substrates (being careful not to remove any underlying material from the substrate) or prepare in the laboratory from liquid samples. For the laboratory preparation, flow some of the well-mixed sample onto a clean glass plate. The use of a paint draw-down bar is recommended to obtain a uniform film thickness not exceeding 2 mils (50 pm). Allow the film to dry in an oven at 105C for a minimum of I h. Scrape the dried film off the glass plate, preferably with a single-edge razor blade. 9.3 Place the flasks containing the liquid coating on the hot plate and slowly increase the temperature until the material is dried. 9.4 When the sample appears to be dry, or when starting with a dried film, gradually increase the temperature of the hot plate until the material chars. 9.5 After charring appears complete, place the flasks in the muffle furnace and ash at 500C. When the ashing appears to be complete (approximately 1 to 2 h), remove the flasks from the muffle furnace and allow to cool to room temperature. 9.6 Carefully add 40 mL of concentrated HO and 8 drops of SnCl2 solution to each flask. Connect the flasks to water-cooled condensers and reflux for 1 h. 9.7 Filter each digested specimen through medium-po rosity filter paper into a 100-mL volumetric flask. If the filtrate is not clear, refilter through fine-porosity filter paper. Rinse each flask several times with water, adding the rinsings to the filter paper. Wash the filter paper several times with water. Adjust the volume to 100 mL with water and mix. 9.8 Aspirate each test solution and determine the absorbance in the same manner in which the instrument was calibrated (see Notes 1 and 2). Determine the concentration of antimony in micrograms per millilitre from the calibra tion curve. If the absorbance is above the range covered by the calibration curve, dilute an aliquot of the test solution to a suitable volume with water containing 40 mL of HCI and 8 drops of SnCl2 solution per 100 mL. If the absorbance is below the range covered by the calibration curve, repeat the analysis using a larger specimen size. N67' 5--Increased sensitivity may be obtained with instruments possessing scale expansion and concentration readout capability. N45' 6--The method of standard additions may be used to improve the accuracy of the analysis. This method is particularly recommended for use with unknown samples where matrix effects may be potentially significant For a detailed description of the procedure and calculations used in the method of standard additions, consult a standard text on atomic absorption spectroscopy or the instruction manual provided by the instrument manufacturer. il :i 549 DUP05 02 97730 D 3717 10. Calculation 10.1 Calculate the mean concentration of antimony in the nonvolatile portion of the sample as follows: Antimony, ppm (mg/kg) in nonvolatile = (Cxfx 104)/(JVKxS) where: C - concentration of antimony in the aspirated test solution, jrg/mL, F = dilution factor from 9.8 (volume diluted to/volume of aliquot), NV ~ percent nonvolatile of paint sample (use 100 if sample was dried film), and S -- grams of sample. 11. Report 11.1 Report the antimony content of the nonvolatile content of the sample and whether the analysis was con ducted on a liquid coating or a dried film. 5Supporting data are available from ASTM Headquarters. Request RR: DOl-lOl 1. 12; Precision and Bias5 12.1 The precision estimates are based on an inter laboratory study in which eight different laboratories ana[ lyzed in duplicate, on two different days, three samples of water-reducible paints and three samples ofsolvent-reducible paints containing from 50 to 200 ppm (mg/kg) antimony The within-laboratory coefficient of variation was found t0 be 4.8 % relative at 31 degrees of freedom and the betweenlaboratory coefficient of variation was 8.8 % relative at 25 degrees of freedom. Based on these coefficients, the following criteria should be used forjudging the acceptability of result at the 95 % confidence level: 12.1.1 Repeatability--Two results,-each the mean of duplicate determinations, obtained by the same operator on different days, should be considered suspect if they differ by more than 14 % relative. 12.1.2 Reproducibility--Two results; each the mean of duplicate determinations, obtained by operators in different laboratories, should be considered suspect if they differ by more than 26 % relative. 12.2 Bias--The mean of duplicate determinations within any laboratory should be within 18 % relative of true value. 13. Keywords 13.1 AAS, antimony; low concentration of antimony in paints The American Society for Testing and Materials takes noposition respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised (hat determination ol the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. Des \ Scope S t.l This j content of : range betwe I coatings or substrates. ' : could not b appropriate ; reagent qua 1.2 This \ safety prob \ responsibih \ priatesafet \ bility of re, statements This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited eitherforrevision ofthis standard or (or additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel f/iaf your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7976 Race St., Philadelphia, PA 79703. 2. Referen 2.1 AS! I D1193 : D2832 Conte j 3. Sumnre | 3.1 Th for analy with pot: tetrafluoi at an ele [ digestion | troscopy. 4. Signifi 4.1 Th | coatings j. This test [ determin l both wa compliar 550 1 'Thiste E and Relate; E mittee DOl I Current K Originally i 1; 2 Annua ft 3 Annua DUP050297731 nteranaes of icible lony. nd to veenat 25 )wing esults )f duor on fer by an of Ferent fer by within value. my in I> i\- Designation: D 3718 - 85a (Reapproved 1991)c1 Standard Test Method for Low Concentrations of Chromium in Paint by Atomic Absorption Spectroscopy1 This standard is issued under the fixed designation D 3718; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. N89' --Keywords were added editorially in July 1991. 1. Scope 1.1 This test method covers the determination of the content of chromium (including chromium oxide) in the ,ange between 0.005 and 1.0 % present in the solids of liquid coatings or in dried films obtained from previously coated substrates. There is no reason to believe that higher levels could not be determined by this test method, provided that appropriate dilutions and adjustments in specimen size and jeagent quantities are made. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. Specific hazard statements are given in Section 7. 1. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water12 D 2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings3 }. Summary of Test Method 3.1 The sample of liquid coating or dried film is prepared for analysis by dry ashing at 50GC followed by digestion with potassium permanganate and sulfuric acid in a polytetrafluoroethylene (PTFE)-lined acid decomposition vessel at an elevated temperature. The chromium in the filtered digestion mixture is determined by atomic absorption spec troscopy. 4. Significance and Use 4.1 The permissible level of heavy metals in certain coatings is specified by governmental regulatory agencies. This test method provides a fully documented procedure for determining low concentrations of chromium present in both water- and solvent-reducible coatings to determine compliance. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 31 and Nov. 29, 1985. Published January .1986. Originally published as D 3718 - 78. Last previous edition D 3718 - 84. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.01. 5. Apparatus 5.1 Atomic Absorption Spectrophotometer, consisting of an atomizer and either a single- or three-slot burner; gas pressure-regulating and metering devices for nitrous oxide (N20) arid acetylene; a chromium hollow cathode lamp with a regulated constant current supply; a monochromator and associated optics; a photosensitive detector connected to an electronic amplifier; and a readout device. 5.2 Muffle Furnace, maintained at 500 10C. 5.3 Force-Draft Oven, maintained at 105 2C. 5.4 Acid Decomposition Vessel, with PTFE digestion cup.4 5.5 Hot Plate, with variable surface temperature control over the range from 70 to 200C. 5.6 Volumetric Flasks, 50, 100 and 1000-mL. 5.7 Pipets, 5, 10, 15, and 20-mL capacity. 5.8 Filter Paper, ashless, medium filtering 15-cm. 5.9 Paint Shaker. 5.10 Crucibles, wide form, porcelain, approximately 30mL capacity.5 5.11 Mortar and Pestle. 5.12 Paint Draw-Down Bar. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Chromium Standard Stock Solution (1 mg/mL)-- 4 Add decomposition cup manufactured by the Parr Instrument Co., 211 Fifty-third St., Moline, IL 61265 (Catalog Number 4745) has been found satisfactory for this purpose. 3 Coors No. 25007 crudbles, or equivalent, have been found satisfactory for this purpose. 6 "Reagent Chemicals, American Chemical Sodety Specifications," Am. Chem ical Soc., Washington, DC. For suggestions,on the testing of reagents not listed by the American Chemical Sodety, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." DUP050297732 D 3718 Dissolve 3.735 g of potassium chromate (K2Cr04) in 100 mL of water and dilute to 1 L. 6.4 Chromium Standard Working Solution (0.1 mg/ mL)--Pipet 10 mL of the chromium standard stock solution into a 100-mL volumetric flask and dilute to volume with water. 6.5 Oxidizing Solution--Dissolve 0.2 g of potassium permanganate (KMn04) in 100 mL of H2S04 (1+1). Stir until completely dissolved. The color of this solution is dark brown. 6.6 Reducing Solution--Dissolve 1 g of hydroxyiamine hydrochloride (NH2OH HC1) in 100 mL of water. 6.7 Reagent Blank--Pipet 5 mL of oxidizing solution into 25 mL of water contained in a 50-mL volumetric flask. Add reducing solution dropwise until the permanganate color has been discharged; then dilute to 50 mL with water. 6.8 Sulfuric Acid (1+1)--Carefully add 1' volume of concentrated H2S04 (spgr 1.84) to 1 volume of water. 6.9 Sulfuric Acid (5 % volume per volume)--Carefully add 50 mL of concentrated H2S04 (sp gr 1.84) to 500 mL of water and dilute to 1 L. 7. Hazards 7.1 Use care in handling concentrated H2S04 because it is corrosive and may cause severe bums of the skin or eyes. Refer to suppliers' Material Safety Data Sheet 7.2 The National Institute for Occupational Safety and Health has stated that hexavalent chromium compounds are hazardous to health. Care should be exercised in preparation of a sample for test. The wearing of a respirator and rubber or synthetic gloves is recommended. In case of contact, wash thoroughly with soap and water. Mixtures containing hexavalent chromium compounds should not be flushed down a drain but disposed of as hazardous waste. 7.3 Use only a rubber bulb aspirator for pipetting liquids. 8. Calibration and Standardization 8.1 Prepare 50-mL quantities of at least four standard solutions bracketing the expected chromium concentration in the sample to be tested. To suitable aliquots of the 100-ppm chromium standard working solution, add 10 mL of the oxidizing solution with a pipet, followed by the dropwise addition of reducing solution until the per manganate color has been discharged, then dilute to 50 mL with water. 8.2 Operational instructions for atomic absorption spectrophotometers vary with different models. Consult the manufacturer's literature for establishing optimum condi tions for the specific instrument used. 8.3 Turn the instrument on and set the wavelength to the 357.9-nm chromium line. Apply the recommended current to the chromium hollow-cathode lamp. Allow the instru ment to warm up for about 15 min and set the slit width. Adjust the nitrous oxide and acetylene pressures and ignite the burner according to instructions. 8.4 Aspirate water to rinse the atomizer chamber. Aspi rate a standard solution and make any necessary readjust ment in instrument parameters to obtain maximum absorp tion. Zero the instrument while aspirating reagent blank solution (6.7). Aspirate each of the appropriate standard solutions and record the corresponding instrument readings. Aspirate water between each standard. 8.5 Transfer a 25-mL aliquot from each of the standard solutions prepared in 8.1 to 50-mL volumetric flasks anjj dilute to volume with water. Repeat the steps outlined in 8.4 for the diluted aliquot solutions. 8.6 Construct a calibration curve on linear graph paper by plotting the absorbance versus concentration (micrograms per millilitre) for each set of standard solutions. N:;' 1--To obtain maximum accuracy one should complete caK, bration and standardization just prior to sample analysis. 9. Procedure 9.1 If the sample is a liquid coating, mix it until homog. neous, preferably on a mechanical paint shaker. Determine the nonvolatile content in accordance with Guide D 2832. 9.2 Determine the ash content of the material under test in duplicate. 9.2.1 Weigh to the nearest 0.1 mg approximately 5 g of liquid coating or 3 g of dried film into each of two tared porcelain crucibles. N<=' 2--Recover dried paint films from previously coated sub strates (being careful not to remove any underlying material from the' substrate) or prepare in the laboratory from liquid samples. For the laboratory preparation, flow some of the well-mixed sample onto a clean glass plate. The use ofa paint draw-down bar is recommended to oblaih a uniform film thickness not exceeding 2 mils (50 pm). Allow the film tedry in an oven at 105"C for a minimum of 1 h. Scrape the dried film oft the glass plate, preferably with a single-edge razor blade. 9.2.2 Place the crucibles containing the liquid coating on the hot plate and slowly increase the temperature until the material is dried. With some types of coatings, an initial:' oven-drying at 105C may be necessary to remove solvents without incurring losses due to spattering. 9.2.3 When the specimen appears to be dry, of when starting with a dried film, gradually increase the temperature of the hot plate until the material chars. 9.2.4 After charting is complete, place the crucibles in the muffle furnace and ash at 500"C. 9.2.5 When the ashing appears to be complete (approxi mately 1 to 2 h), remove the crucibles from the muffle furnace and allow to cool to room temperature in a desiccator. Weigh and calculate the mean value for the percent ash. 9.3 Transfer each ash to a clean, dry mortar and grind to a fine, uniform powder. Weigh to the nearest 0.1 mg, 0.02 to 0.2 g of each ash directly into separate decomposition vessel inserts. N:;' 3--For a material containing 50- ppm <mg/kg) of chromium based on the solids and having 50 % ash and 70 % nonvolatile material, 0.2 g of ash extracted and diluted to 50 mL will contain 0.28 pg of chromium per millilitre, and for one containing 10 000 ppm, 0.02 g of ash extracted and diluted to 100 mL will contain 2.8 jrg of chromium per millilitre. To ensure complete recovery of chromium, do not use more than 0.05 g of ash for materials that are known or suspected to contain over 1000 ppm of chromium based on the solids. 9.4 Pipet exactly 10 mL of oxidizing solution into the cup. Swirl gently to facilitate mixing. Place , the vessel in a circulating oven at 105C for IV2 h. 9.5 Remove the vessel from the oven and allow to cool slowly to ambient temperature. Do not cool by placing the vessel in a refrigerator or freezer, or by submerging it in a cot fur r sho StnE c dir dig ins sev drc un' dil' t sor cal mi' cui cal sui rep ] the me pot cai< stai ma 10 tht ' Ch : wfc C F1 552 DUP0502 97733 ie standard flasks and lined in 8.4 )h paper by nicrograms omplete cali- til homogeDetermine e D 2832. ; under test ttely 5 g of f two tared coated subrial from the pies. For the ; onto a clean ded to obtain jw the film to dried film off coating on re until the , an initial ve solvents or when imperature ibles in the e (approxihe muffle ure in a e for the grind to a g, 0.02 to ition vessel of chromium ttiie material, n 0.28 jig of pm, 0.02 g of of chromium 1, do not use suspected to ito the cup. /essel in a ow to cool placing the jing it in a D 3718 cooling liquid. When cooled, carefully unseal the vessel in a fyjjie hood. M>?' 4--When the vessel is disassembled, if the solution does not jftov/ the presence of excess permanganate, repeat the digestion using a smaller weight of ash. 9.6 Quantitatively filter the contents through filter paper directly into a 50 or 100-mL volumetric flask. Rinse the digestion cup several times with water, transferring any insoluble material to the filter paper. Wash the filter paper several times with small volumes of water. Add hydroxylamine hydrochloride solution dropwise to the filtrate until the permanganate color has been discharged, then dilute to volume with water. 9.7 Aspirate each test solution and determine the ab sorbance in the same manner in which the instrument was calibrated. Determine the concentration of chromium in micrograms per millilitre from the appropriate calibration curve. If the absorbance is above the range covered by the calibration curve, dilute an aliquot of the test solutions to a suitable volume with H2S04 (5 % volume per volume) and repeat the determinations. N@A' 5--The method of standard additions may be used to improve the accuracy of the analysis. This test method is particularly recom mended for use with unknown samples where matrix effects may be potentially significant. For a detailed description of the procedure and calculations used in the method of standard additions, consult a standard text on atomic absorption spectroscopy or the instruction manual provided by the instrument manufacturer, 10. Calculation 10.1 Calculate the mean concentration of chromium in the nonvolatile portion of the sample as follows: Chromium, ppm (mg/kg) in nonvolatile = (CxFx Ax V)/(S x NV) where: C = concentration of chromium in the aspirated test solution, jig/mL, F = dilution factor from 9.7 (volume diluted to volume of aliquot), A = mean percent ash as determined in 9.2.5, V = volume diluted to in 9.6 (50 or 100 mL), S = weight of ash, and NV = percent nonvolatile of paint sample (use 100 if sample was a dried film). 11. Report 11.1 Report the chromium content of the nonvolatile portion of the sample tested and whether the analysis was conducted on a liquid coating or a dried film. 12. Precision and Bias7 12.1 The precision estimates are based on an inter laboratory study in which six different laboratories analyzed in duplicate, on two different days, four samples of waterreducible paints and four samples of solvent-reducible paints containing from 50 to 10 000 ppm (mg/kg) chromium. The within-laboratory coefficient of variation was found to be 4.9 % relative at 39 degrees of freedom and the betweenlaboratory coefficient of variation was 8.5 % relative at 31 degrees of freedom. Basal on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 12.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 14 % relative. 12.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 24 % relative. 12.2 Bias--The mean of duplicate determinations within any laboratory should be within 17 % relative of true value. 13. Keywords 13.1 AAS, chromium; low concentration of antimony in paints 'Supporting data are available from ASTM Headquarters. Request RR: D01-10IZ The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revisedeither reapproved or withdrawn. Your comments are Invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. V you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050297734 < Designation: D 3719 - 87 |- Standard Test Method for Quantifying Dirt Collection on Coated Exterior Panels1 v^here: =ar ^*B -- ar This standard is issued under the fixed designation D 3719; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon <) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers an instrumental procedure for quantifying the degree of dirt collection on exposed exterior coated panels. 1.2 This test method is limited to those coated exterior panels with lightness values before exposure greater than that of dirt, that is, above a value of 52. 1.3 The instrumental readings do not distinguish between dirt collection and mildew growth. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents are used to establish that dirt collection is the primary cause of such a change, this test method can be used to quantify the degree of dirt collection or, more properly, the degree of change in visual appearance of the coated surface due to dirt collection. - 5.2 When used in this manner and with color change, exposure duration and environment specified, this test method can provide a performance specification with respect to"dirt collection. 6. Apparatus and Materials 6.1 Color Difference Meter, complying with Method D 2244. 6.2 Test Panels, of any convenient size and of substrate suitable for exterior use. jO- Repor 10.1 Re 10.1.1 , value, and 35 well as exposed p value. 10.1.2,. other that 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates2 D 3274 Test Method for Evaluating Degree of Surface Disfigurement of Paint Films by Microbial (Fungal or Algal) Growth or Soil and Dirt Accumulation2 3. Definition 3.1 dirt collection--the deposit of foreign matter con sisting of dirt, soot, or stain present on the surface ofexposed exterior coated panels. 3.1.1 This test method measures total dirt collection. Loose dirt may be washed and removed from specimens if only imbedded dirt collection is to be measured. 4. Summary of Test Method 4.1 Lightness readings using a color difference meter are made before and after exposure, and the difference is considered to be due to dirt collection. 5. Significance and Use 5.1 Change in color or appearance of coated exterior surfaces due to such factors as dirt collection or retention is undesirable. If Test Method D 3274 or other test methods * This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.52 on Factory-Coated Wood Products, Current edition approved Oct. 30, 1987. Published December 1987. Originally published as D 3719 - 78. Last previous edition D 3719 - 80. 2 Annual Book ofASTM Standards, Vol 06.01. 7. Preparation of Test Panels 7.1 Apply the material under test to the test panels in accordance with Test Method D823, or as agreed upon between the purchaser and the seller. Allow the final coat of air drying systems to cure for 7 days before, exposure. i 8. Procedure 8.1 Operate the color difference meter in accordance with the manufacturer's instructions. Standardize with either a primary or working standard as defined in Test Method D 2244. Restandardize at sufficient intervals, in accordance [ with the manufacturer's instructions, to minimize the effects 1 of instrumental drift. 1 8.2 Determine the metric lightness, L*, in the CIE 1976 L*a*b* Uniform Color Space (CIE LAB), for each unex posed panel at three marked, random locations. Calculate the arithmetic mean, L*A. 8.3. Expose the panels at a 45. angle to the horizontal facing the equator at an exterior location for 61 days. 8.3.1 The calendar time, location, angle of exposure, orientation, exposure time, and method of exposure may be modified by mutual agreement. 8.4 Remove the panels and determine, using the proce- i dure outlined above, the percent light reflectance value, L*, for the exposed panels. Calculate the arithmetic mean of the | marked locations, L*B. | 9. Calculations 9.1 Compute the dirt collection index, Dc, as follows: 554 ------------------------------------------------------------ -- : _. Jk_. DUP050297735 f cause tify the >ree of to dirt hange, is test respect lethod ostrate 0 3719 Dc = ^x 100 where: \*K = arithmetic mean of unexposed panel values, and j/B = arithmetic mean of exposed panel values. jO. Report 10.1 Report the following information: 10.1.1 Arithmetic mean and range of each panel's Lx value, and whether fungal growth is included in the reading, as well as the calculated dirt collection index. Report if the exposed panel was washed before taking the light reflectance value. 10.1.2 Any noticeable color change which, for reasons other than dirt accumulation, may have occurred. The dirt collection index is not valid if these color changes or fungal growth are significant. 10.1.3 Description of the method of panel preparation, including substrate identity, coating types, number of coat ings used, methods of application, coverage, and drying conditions. 10.1.4 Description of the exposure conditions including location and calendar time of exposure period. 10.1.5 Identification of the color difference meter by manufacturer's name and code number. 10.1.6 Which Adams color scale was used. 11. Precision and Bias 11.1 Precision--Precision of the dirt collection index has not been determined but the precision of the lightness values used in its calculation has been defined. 11.2 Bias--Bias cannot be determined. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is sub/ect'to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, PA 19103. lels in upon oat of a with her a athod lance ffects 1976 inexaulate :ontal asure, DUP050297736 t Designation: D 3723 - 84 (Reapproved 1990)1 Standard Test Method for Pigment Content of Water-Emulsion Paints by LowTemperature Ashing1 This standard is issued under the fixed designation D 3723; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<} indicates an editorial change since the last revision or reapproval. I -p = 5= i 6A * desic , 7- C I 7. " NBC' --Section 9 was added editorially in May 1990. 1. Scope 1.1 This test method covers a procedure for the pigment content determination of water-based paints. It is' applicable only to pigments that do not decompose or lose weight at temperatures below 500C. Such pigments include most metal oxides, silicates, and a majority of anhydrous inor ganic salts. 1.2 Many water-based paints contain pigments and or ganic colorants that lose water of hydration or decompose at this temperature. The residual ash should be carefully inspected for changes in color or texture that could indicate a pigment alteration and hence lead to erroneous results. Caution should therefore be exercised when applying this test method to samples containing unknown pigment composi tions. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification for Reagent Water2 3. Significance and Use 3.1 This test method is used by paint producers and consumers for product process control and for product acceptance. 4. Apparatus 4.1`- Oven, forced draft, maintained at 105 2C. 4.2 Furnace, muffle, maintained at 450 25C. 4.3 Svringe, 5-mL. 4.4 Aluminum Foil Dish, 58 mm in diameter by 18 mm high with a flat bottom. The bottom.of the dish should be as nearly flat as possible so that a uniform film is produced. 5. Reagents 5.1 Purity ofReagents--Reagent grade chemicals shall be wtae C* used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem- ; B* 5 -- ical Society, where such specifications are available.3 Other ; .grades may be used, provided it is first ascertained that the 8 reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 5.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type III of Specification D 1193. 5.3 Ammonium Hydroxide 4--Add 1 volume of concen trated NH4OH (sp gr 0.90) to 3 volumes of water. i lat tor tin lat ab B 6. Procedure I sh 9f 6.1 Mix samples until homogeneous, preferably on a I mechanical shaker. If air bubbles become entrapped in a 1 sample, stir it by hand. 6.2 Draw approximately 1.5 g of the test paint into a R: 5-mL syringe and weigh to 1 mg. Add the paint dropwise (about 30 drops) into a tared-aluminum foil dish that con tains 2 mL of water (5.2). Swirl the dish during the addition and continue the swirling until the specimen is completely dispersed. Reweigh the syringe to 1 mg. Transfer between 0.4 and 0.6 g of sample to the dish. If not, adjust the transferred volume and prepare a new specimen. If the specimen ag glomerates or forms a lump that cannot be dispersed, a drop or two of ammonia (5.3) may facilitate the dispersement. If the lumping persists, discard the specimen and prepare a new one. Prepare a duplicate specimen in the same manner. 6.3 Dry the specimen and dishes in the 105 2C oven for a minimum of 1 h after making certain that the dishes are level. Ifthe coating does not uniformly cover the bottom of a dish, prepare a new specimen and repeat. NDE' --The percent nonvolatile content, N, at 105C may be determined by drying dishes to constant weight and calculating as follows: N = ^-^xl00 (1) where: A - weight of dish and specimen after heating, : :l 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Oct. 26, 1984. Published January 1985. Originally published as D 3723 - 78. Last previous edition D 3723 - 78. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3"Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." * For guidance in the safe handling of ammonium hydroxide consult the Manufacturing Chemists Association's Chemical Safety Data Sheet. j |j 556 DU PO 502 97737 D 3723 ltended ; of the Chem3 Other :hat the without refert water oncen- ' on a :d in a into a opwise at conddition ipletely sen 0.4 sferred ten agx drop :nt. If i new | g a weight of dish atone, and S ^ = specimen weight. I 6.4 Transfer the dishes to a muffle furnace and heat at 450 1 j. 25C for 1 h. Remove from the furnace, cool in a jesiccator and weigh. ^ Calculation 7.1 Calculate the percent pigment content, P, as follows: P = x 100 (2) tfhere: q * weight of the dish and specimen after ignition in the furnace, g = weight of the dish alone, and 5 = specimen weight. g. Precision and Biass g. 1 Precision: Pigment Content--On the basis of an interlaboratory test of this test method in which eighteen opera tors in nine laboratories analyzed three materials containing three pigment levels between 24 and 28 %, the withinlaboratory standard deviation was found to be 0.24 % absolute and the between-laboratories 0.38% absolute. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 5 Supporting data are available from ASTM Headquarters. Request RlfcDOl.lOM. 8.1.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 0.66 % absolute. 8.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 1.05 % absolute. 8.2 Bias: Pigment Content--On the basis of the same study, the mean of two determinations should be within 5 % relative of the formula pigment content of a waterborne paint containing only inorganic pigments. 8.3 Precision: Nonvolatile Content-- On the basis of an interlaboratory test of this test method in which fourteen operators in seven laboratories analyzed three materials containing three nonvolatile levels between 43 and 48 %, the within-laboratory standard deviation was found to be 0.18 % absolute and the between-laboratories standard deviation was found to be 0.445 % absolute. Based on these standard deviations,the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 8.3.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 0.49 % absolute. 8.3.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 1.23 % absolute. 9. Keywords 9.1 low-temperature ashing; pigment content; water emul sion paints The American Society for Testing andMaterials takes no position respecting the validity ofany patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you fee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards,. 1916 Race St., Philadelphia, PA 19103. oven as are n of a nay be iting as (1) a. Chemlistedby irds," by ed States isult the 557 DUP05 02 97738 Designation: D 3730 - 78 (Reapproved 1088)'61 An American National Standard Standard Guide for Testing High-Performance Interior Architectural Wall Coatings1 This standard is issued under the fixed designation D 3730; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval A superscript epsilon (<) indicates an editorial change since the last revision or reapproval il NFG' --Editorial changes were made throughout, including the title, in October 1988. 1. Scope 1.1 This guide covers the selection and use oftest methods for high-performance interior architectural wall coatings (HIPAC) that differ from more conventional coatings in that they are tougher, more stain-resistant, more abrasion-re sistant and, ordinarily, designed to be applied to wall surfaces of steel, masonry (poured concrete, concrete block, or cinder block), and plaster or gypsum wallboard. The tests that are listed in Tables 1 and 2 are designed to measure performance properties. These tests may not all be required for each HIPAC system. Selection of the test methods to be followed must be governed by experience and the requirements in each individual case, together with agreement between the purchaser and the seller. 1.2 High-performance architectural coatings are tough, extra-durable organic coating systems that are applied as a continuous (seamless) film and that cure to a hard finish. The finish can be high gloss, semigloss, or low gloss as desired. These coatings are resistant to persistent heat, humidity, abrasion, staining, chemicals, and fungus growth. They are used in areas where humidity, wear, or unusual chemical resistance requirements, particularly to soiling, are required and where strong detergents are used to maintain sanitary conditions. Halls and stairways in public buildings, lavatories, stall showers, locker areas, animal pens, and biological laboratories are typical applications. In addition, food processing plants, dairies, restaurants, schools, and transport terminals frequently use HIPAC systems. These are effective in many areas of building interiors compared with tile and are of low materials and maintenance costs. HIPAC systems should be used as a complete system only as recommended by the manufacturer since the individual coats in a system are formulated to be compatible with each other. HIPAC systems should be applied only to properly prepared surfaces such as steel and masonry that includes cinder blocks and cement blocks. They can be applied over plaster and gypsum wallboard. Ordinarily, a prime or fill coat, if required, is part of the system. 1.3 While they are excellent for walls, HIPAC are not usually intended for ceilings and floors. They would not ordinarily be used in homes, although parents with small children might want to use HIPAC coatings on some walls. 1 This method is under the jurisdiction of ASTM Committee D-l on Faint and Related Coatings and Materials, and is the direct responsibility of Subcommittee DO 1.42 on Architectural Finishes. Current edition approved Dec. 21, 1978. Published January 1979. 1.4 The types or resin ordinarily used are the following; epoxy-polyamide, two-package; polyester-epoxy type, two. package; polyurethane, one-package or two-package. However, other resin types are not excluded provided they can meet the requirements (performance specifications) laid down by the purchaser. 1.5 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see the Note in 7.5. 2. Referenced Documents 2.1 ASTM Standards: C 220 Specification for Flat Asbestos-Cement Sheets2 D 16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products3 D93 Test Methods for Flash Point by Pensky-Martens Closed Tester4 D185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints5 D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts6 D 523 Test Method for Specular Gloss6 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer6 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels6 D 1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers6 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base6 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems6 D1211 Test Method for Temperature-Change Resistance ofClear Nitrocellulose Lacquer Films Applied to Wood6 2 Annual Book ofASTM Standards, Vol 04.05. 3 Annual Book ofASTM Standards, Vols 06.01, 06.02, and 06.03. 4 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 5 Annual Book ofASTM Standards, Vols 06.01 and 06.02. 6 Annual Book ofASTM Standards, Vol 06.01. 558 D 1212 of a D 1296 Dilu- D 1308 on C D 147f quer D 164* nish D 172' of C D224 fror D224 in ' D261 Ur< D27` Efl D281 by D28 Ri D3C to R D3: th c E 8B E9 4 1 E: 2.2 21 21 21 3( 4: 4 41 4. 4` 4; 6 6 6 2 1 20C DU P050297739 itional Standard 'ollowing: /pe, twoge. How. they can 3ns) laid tls, operurport to use. It is establish nine the ' For a 3tS2 acquer, Martens sments, intsby g the fonn ts on /-Film s6 ent of oplied f Pigtance 7ood6 # D 3730 p 1212 Methods for Measurement of Wet Film Thickness of Organic Coatings6 p 1296 Test Method for Odor of Volatile Solvents and Diluents7 p 1308 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes6 p 1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products6 pl644 Test Methods for Nonvolatile Content of Var nishes8 p 1729 Practice for Visual Evaluation of Color Differences of Opaque Materials8 P2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates6 D2247 Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity6 D2615 Test Method for Free Toluene Diisocyanate in. Urethane Polymers by Distillation9 D2794 Test Method for Resistance of Organic Coatings to Effects of Rapid Deformation (Impact)6 D2801 Test Method for Leveling Characteristics of Paint by Draw-Down Method10 D2805 Test Method for Hiding Power of Paints by Reflectometry6 D 3023 Practice for Determination of Resistance of Fac tory-Applied Coatings on Wood Products to Stains and Reagents6 D 3273 Test Method for Resistance to Growth of Mold on the Surface of Interior Coatings in an Environmental Chamber6 E 84 Test Method for Surface Burning Characteristics of Building Materials11 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry12 E 300 Practice for Sampling Industrial Chemicals13 2.2 U.S. Federal Test Methods Standard 141:14 2112 Application by Roller 2131 Application of Sprayed Films 2141 Application of Brushed Films 3011 Condition in Container 4121 Dry Opacity 4122 Hiding Power (Contrast Ratio) 4203 Reducibility and Dilution Stability 4250 Color of Pigmented Coatings 4494 Sag Test (Multinotch Blade) 4541 Working Properties and Appearance of Dried Film 6141 Washability of Paints 6142 Scrub Resistance 6192 Abrasion Resistance (Taber Abraser) 2.3 U.S. Federal Specification:14 TT-F-I098 7 Annual Book ofASTM Standards, Vol 06,03. 8 Annual Book ofASTM Standards, Vol 14.02. 9 Discontinued, see 1979 Annual Book ofASTM Standards, Part 28. 10 Discontinued; see 1989 Annual Book ofASTM Standards, Vol 06.01. 11 Annual Book ofASTM Standards, Vol 04.67. 12 Annual Book ofASTM Standards, Vols 06.01 and 14-.02. 13 Annual Book ofASTM Standards, Vols 06.03 and 15.05. 14 Available from Standardization Documents Order Desk, Bldg. 4, Section D, TOO Robbins Ave., Philadelphia, PA 19111-5094. 2.4 Military Standards:14 MIL-C-83286, Determination of Free Aliphatic Diiso cyanate Monomer by Infrared Spectroscopy 3. Definitions 3.1 For definitions of terms used in these practices, refer to Definitions D 16. 4. Conditions Affecting Performance of HIPAC Coating Systems 4.1 Practical requirements for high performance coatings may vary with: 4.1.1 Substrate type such as concrete, poured or precast block, lime-gypsum plaster, etc. 4.1.2 Climatic conditions, both generally and specifically, at the time of coating application. ASTM standard condi tions for laboratory testing are 73.5 3.5F (23 2C) and 50 5 % relative humidity. 5. Sampling 5.1 Prior to sampling, establish the condition of the container since damage to it may cause evaporation, skin ning, or other undesirable effects. Excessive storage time and temperature fluctuations may cause settling or changes in viscosity. 5.2 Sample the coating in accordance with the Practice E 300. Determine the weight per gallon or kilogram per litre in accordance with Test Method D 1475 and repeat until two successive readings agree within 0.2 lb (90 g) or as agreed upon between the purchaser and the seller. Samples for testing may then be taken. 5.3 Specify the amount of the sample, the package sizes, and identification codes to assure a representative sample. A 1-gal (3.8-L) sample is usually sufficient for the recom mended tests but the practice gives sample size in relation to quantity and size of container. 6. Laboratory Tests 6.1 Preparation of Test Panels: 6.1.1 Unless otherwise specified, test panels shall be \xh by 71/2 by 15!/2-in. (38 by 190 by 395-mm) masonry units made from either standard lightweight concrete block, having an apparent specific gravity of 1.60 to 1.62 or smooth asbestos cement board complying with Specification C 220. 6.1.2 One face only of the test panel shall be coated with the complete system, in a vertical position. For concrete, the filler shall either comply with U.S. Federal Specification TT-F-1098 or be the. material specified and supplied by the manufacturer. The filler coat shall be applied in conform ance with the manufacturer's printed directions for surface preparation, mixing, application, coverage, and curing time under standard conditions of temperature and humidity. 7. Liquid Coating Properties 7.1 Condition in Container--Thickening, settling, and separation are undesirable and objectionable if a coating, after storage, cannot be readily reconditioned and made suitable, for application with a reasonable amount of stirring. The referenced method covers procedures for determining changes in. properties after storage. Determine the condition in the container in accordance with Method 3011 of Federal 559 DUP050297740 # D3730 t TABLE 1 List of Test Methods by Properties Test Method Liquid coating properties: Condition in container Coarse particles and foreign matter Density or weight per gallon Fineness of dispersion Odor Consistency Dilution stability Flash point Free diisocyanate content Volatile content Application and film formation: Application by brush Application by roller Application by spray Leveling properties Working properties Sag resistance Wet film thickness Producing films of uniform thickness Curing time Appearance of dry coating: Color difference, visual Color difference, instrumental Directional reflectance Gloss (60-deg specular) Hiding power Properties of dry coatings: Abrasion resistance Adhesion , Chemical resistance Coating thickness Flame spread test Fungus resistance Heat and coal resistance Heat and tumidity resistance Impact resistance Perspiration resistance Scrubbability Washability * Modified. Section 7.1 7.2 7.3 7.4 7.5 7.6 7.7 7.8 7.9 7.10 8.1 8.2 8.3 8.4 - 8.5 8.6 8.7 8.a 8.9 9.1 9.1 9.2 9.3 9.4 10.1 10.2 10.3 10.4 10.5 10.6 10.7 10.8 10.9 10.10 10.11 10.12 ASTM Test Method D185, Section C D1475 01210 D1296 D 662 D 93 D 2615 D 1644 D2801 D1212 D 823 D2244 E 97 D523 D344 D1308* D 1005,0 1186 E 85 D 3273 D 1211* O 2247* D 2794 Federal Test t Standard No. nf 3011 4203 2141 2112 2131 4541 4494 4250 4121-4122 6192 6142 6141 ^ Test Method Standard No. 141. 7.2 Coarse Particles and Foreign Matter--Coatings must be free of oversize particles and foreign matter to form a uniform film of good appearance, a typical maximum being 0.5 weight % of total coating. The specified test with a No. 325 (45-jim) screen gives the percent of these particles in a material. Determine coarse particles and foreign matter in accordance with Test Methods D 185, Section G. 7.3 Density or Weight Per Gallon--The density of a coating as measured by weight per gallon is used to assure product uniformity from batch to batch and provides a check against the theoretical weight calculated from the formula. The referenced test method gives a procedure for measurement of the density of a liquid coating. The density is expressed as weight in pounds per 1 U.S. gal or in kilograms per litre of the coating at a specified temperature. A calibrated weight-per-gallon cup is used. Determine weight per gallon in accordance with Test Method D 1475. 7.4 Fineness of Dispersion--One method for measuring the degree of dispersion is to draw a liquid coating down in a tapered groove in a hardened steel block with a groove varying in depth from 4 to 0 mils (100 to 0 pm). The point at which continuous groupings of particles or agglomerates, or both, protrude through the surface of the wet film is taken as the fineness reading. Lower readings in mils or micrometers or higher readings in Hegman units indicate better disper sion. A typical fineness of dispersion requirement is a reading of 1.5 mil (38 pm) or 5 Hegman for HIPAC. Determine fineness of dispersion in accordance with Test Method D 1210. 7.5 Odor--Adequate ventilation is required as some sol vent combinations produce obnoxious odors. Test for odoi in accordance with Test Method D 1296. NHI' : Warning--Even though the odor may be pleasant, the fumes may be dangerously toxic. 7.6 Consistency--Coatings of a given type should fall within a consistency range agreed upon. In the referenced test method, consistency is defined as the load in grams required to produce a specified rate of shear. A typical range is 85 to 135 Krebs unit (KU) for base coats and 70 to 95 KU for glaze coats. Determine the consistency of the product in accordance with Test Method D 562. 7.7 Dilution Stability--The diluent suggested for reduc tion should be readily incorporated into the coating without excessive stirring or shaking. This test is a measure of the stability of a coating that has been reduced to a desired viscosity, for example, for spray application. Determine Jjasion resis ^esion Implication by ,{,emicai resis ;oarse particl gating thickr |or different dition in c Consistency curing time Density or we Dilution stablli Directional ref ripeness of d rjarne spread :iash point :ree diisocya: rungus resist 3 0I SS (60-dec Heat and colt Heat and hur Hiding power impact resist Leveling prop Odor perspiration i producing fEr Sag resistant Scrubbability Volatile confc Washability dilution s Test Met 7.8 Fh character bustion. often usi carriers, meet fin Occupat ture is : applied accordar cups. 7.9 Ft that diis coatings diisocyai controlk accepted weight, (TD1) ar been she Determi with Tef applicab now bei: can be d U.S. Mi 560 ______ ,_______---------------------------------------- - JG DUP050297741 Method x 141 meters lisper- is a !PAC. Test e solodor : fumes Id fall renced grams range >5KU uct in reducithout of the esired rmine Test Method Abrasion resistance Adhesion Application by brush Application by roller Application by spray Chemical resistance Coarse particles and foreign matter Coating thickness Color difference Condition in container Consistency Curing time Density or weight per gallon Dilution stability Directional reflectance fineness of dispersion fiame spread test Flash point Free diisocyanate content Fungus resistance Gloss (60-deg specular) Heat and cold resistance Heat and humidity resistance Hiding power impact resistance Leveling properties Odor Perspiration resistance Producing films of uniform thickness Sag resistance Scrubbability Volatile content Washability Wot film thickness Working properties ' Modified. w D 3730 TABLE 2 Alphabetical List of Test Methods Section ASTM Test Method 10.1 10.2 8.1 8.2 8.3 10.3 7.2 10.4 9.1 7.1 7.6 8.9 7.3 7.7 9.2 7.4 - 10.5 7.8 7.9 10.6 9.3 10.7 10.8 9.4 10.9 8.4 7.5 10.10 8.8 8.6 10.11 7.10 10.12 8.7 8.5 D1308/1 D185, Section C D1005-D1186 D 2244,D1729 D562 D 1475 E 97 D 1210 E 84 D 93 O 2615 D 3273 D 523 D1211* 0 2247'' D 344 D 2794 D 2801 D1296 0823 D 1644 D 1212 Federal Test Method Standard No. 141 6192 2141 2112 2131 4250 3011 4203 4121-4122 4494 6142 6141A 4541 dilution stability in accordance with Method 4203 of Federal Test Method Standard No. 141. 7.8 Flash Point--Organic solvents used in coatings have characteristic temperatures at which they will support com bustion. This temperature is known as the flash point. It is often used for danger classification in shipment by common carriers. It is also used to determine conditions of storage to meet fire regulations and also the safety requirements of the Occupational Safety and Health Act (OSHA). This tempera ture is not directly translatable as the danger level when applied as films to surfaces. Determine the flash point in accordance with Test Methods D 93, when in closed or open cups--- 7.9 Free Diisocyanate Content--It is generally recognized that diisocyanate vapors from polyurethane-type HIPAC coatings are potential health hazards. Therefore, the free diisocyanate content of urethane coating systems must be controlled at an acceptable maximum level, the present accepted maximum being 0.5 % based on total coating weight, which is applicable only to toluene diisocyanate (TDI) and hexamethylene diisocyanate (HMDI). It has not been shown that this level is applicable to all diisocyanates. Determine free toluene diisocyanate content in accordance with Test Method D 2615. There is no ASTM test method applicable for the other diisocyanates, but test methods are now being developed by ASTM. The presence of free HMDI can be determined by the method described in Appendix I of U.S. Military Specification MIL-C-83286. 7.10 Volatile Content (Weight Percent)--The percent of volatile matter indicates the thinner loss from the film as it dries. Calculate the volatile content of the coating by difference after determining the nonvolatile content in accordance with Test Methods D 1644. S. HIPAC Application and Film Formulation 8.1 Application by Brush--Brushed films should be smooth and free of seeds and on vertical surfaces should show no sagging, color streaking, or excessive brush marks. Test application or brushed films in accordance with Method 2141 of Federal Test Method Standard No. 141. 8.2 Application by Roller--Walls are frequently painted with rollers that produce slight stipple effects. Test roller coating properties in accordance with Method 2112 of Federal Test Method Standard No. 141. 8.3 Application by Spray--Interior coatings are some times applied by spray. Both air and airless spray are used in commercial work. Test in accordance with Method 2131 of Federal Test Method Standard No. 141. 8.4 Leveling Properties--Leveling is a factor in hiding and appearance of coatings. The referenced test method covers the laboratory determination of the relative leveling charac teristics of liquid coatings. Determine leveling property in accordance with Test Method D 2801. ~ 8:5 Working-Properties--Working properties of a coating are generally compared to a standard or described by requirement in the product specification. Test working 561 DUP0502 97742 D 3730 properties in accordance with Method 4541 of Federal Test Method Standard No, 141. 8.6 Sag Resistance--Some coatings sag and form curtains before the film sets. Test for sag resistance in accordance with Method 4494 of Federal Test Method Standard No. 141. 8.7 Wet Film Thickness--Measurement of wet film thick ness is useful in calculating spreading capacity or adjusting application to an agreed upon square feet per gallon or square metres per litre. Determine wet film thickness in accordance with Test Methods D 1212. 8.8 Producing Films of Uniform Thickness--The fol lowing test method covers the preparation of enamel films of uniform thickness essential in conducting various tests. Prepare films in accordance with Test Methods D 823. 8.9 Curing Time--The cure of a HIPAC system is gov erned by the composition of the coating and by atmospheric conditions during cure. Insufficient cure may result in poor stain and abrasion performance. Typical cure times are between 3 and 21 days depending upon the system. There are no applicable ASTM or Federal test methods to measure cure of HIPAC systems, but one method used is as follows: 8.9.1 After the final cure for the duration specified by the manufacturer, place 10 drops of acetone on the coated surface and cover with a 25-mm watchglass. After 3 min lift the watchglass and remove the acetone by blotting. Allow a recovery period of 1 h and examine for evidence of softening or wrinkling of the coating. 9. Appearance of Dry Coating 9.1 Color Difference--Visual comparison of color is fast and often acceptable, although numerical values are not obtained. However, the appearance of a color is greatly influenced,by several factors. 9.1.1 A color next to a yellow wall will look different than the same color next to a blue wall. The same color illuminated by incandescent light, fluorescent light, and natural northern light, will appear to be different because the spectral makeup of the incident lights vary. 9.1.2 Gloss also affects color appearance. The same color with a low gloss and high gloss will usually appear to differ, although instrumentally the colors may be identical. The reason is that the color seen is different when the incident light is unevenly scattered by the rougher surface of the low-gloss finish. Often times, the paint manufacturer is expected ^to produce color matches for all sorts of incident conditions. Hence, the method given in Method 4250 of Federal Test Method Standard No. 141 provides a reason ably accurate method of visual comparison using natural northern light as the incident source. Where a more accurate method of visual comparison is desired,. Practice- D 1729 should be employed since it specifies the composition of the incident light. 9.1.3 Determination of color difference by instrument in accordance with Method D 2244 is the more reproducible, but visual perception is the more nearly related to the needs in actual use,' where the conditions are unpredictable but may be expected to include many types of lighting. 9.2 Directional Reflectance--This is an important prop erty of a white coating as. it is a measure of the brightness of the surface. Frequently the reflectance of a white coating may- be reduced to increase hiding power. To maintain jpice). To 1 brightness, a typical minimum reflectance value of 84 mgv provide a su be specified for white. Determine directional reflectance jn pipe having accordance with Test Method E 97. through wh 9.3 Gloss (60-deg Specular)--Semigloss HIPAC coating, removal of; are particularly sensitive to loss of gloss due to differentia) between the absorption on some surfaces. This is often controlled by occurs betv testing the gloss of a system applied over a nonabsorbeni fional dowe substrate such as glass and an absorbent surface like gypsuij 10.2.2 If board. Determine the specular gloss on appropriate sub, '< panel coate strates in accordance with Test Method D 523. i 73.5 3.5 9.4 Hiding Power: water in cc 9.4.1 Hiding power is a measure of the ability of a coating the end of to hide the substrate. However hiding power of a white Ibf (90 N) coating is inversely related to its reflectance so that j dowels, us decreases with increasing directional reflectance. Hiding 10.3 Cl power is expressed as area covered per unit volume of HIPAC sj coating to produce a reflectance over a black surface that is removal \ 98 % of the reflectance over a white surface (contrast ratio of cleaners, 0.98). method s 9.4.2 Hiding power by contrast ratio can be determined HIPAC s by application of a coating to black and to white glass panels Method or to black and white charts. The former is more accurate weight 9 and is the preferred procedure in Test Method D 2805, chlorite, which also employs automatic film application to eliminate and sulft rheological effects. Method 4122 of Federal Test Method absorben Standard 141 is a less detailed procedure using drawdown with a 2: application on black and on white glass. Contrast ratio oi | to recov black and white charts can also be determined in accordance I with Procedure B of Method 4121. 9.4.3. Hiding power is determined in Test Method D 344 by comparison of brush application of the material under test and a standard coating. | 9.4.4 Determine hiding power by one of the above methods consistent with the degree of importance attached to this parameter. coating' 10.4 ness fro coating D 1186. Method 10.5 should the flar 10. Properties of Dry Coatings 10.1 Abrasion Resistance--Wear resistance of HIPAC coatings is one of the outstanding qualities which distin guishes them from ordinary interior wall and trim enamels. Determine abrasion resistance in accordance with Method 6192 of Federal Test Method Standard No. 141. 10.2 Adhesion--Adhesion is the property of the film that resists removal from the substrate when scuffed or scraped and is an important property in a HIPAC system. There are no applicable ASTM or Federal test methods to measure adhesion of HIPAC systems, but one method used is as follows: 10.2.1 Attach heavy screw eyes to one end of each of twelve 1-in. (25-mm) diameter wood or metal dowels aps proximatelyi 1 Vz in. (38 mm) long. Glue the dowels to the cured coating on a test panel at 3-in. (75,-mm) centers, using a cold-curing epoxy adhesive applied to both the coating and the dowel. Make sure that the button of adhesive does no! extend beyond the diameter of the dowel or the area will be larger than intended. After conditioning for 3 days at 73.5* 3.5F (23 2C), slowly apply an axial pull of 150 lbf (68ff j N) to each of three dowels. The force may be applied by any method having an accuracy of 5 %, such as by a system of weights and pulleys or through a spring scale (spring 562 DUP050297743 'o maintain e of 84 may :flectance in AC coatings ) differential mtrolled by onabsorbent like gypsum update sub- of a coating of a white so that it ice. Hiding volume of rface that is trast ratio of determined glass panels ire accurate od D 2805, to eliminate est Method ; drawdown ast ratio on accordance thod D 344 terial under the above ce attached of HIPAC ich distini enamels, h Method e film that or scraped t. There are to measure used is as of each of dowels apwels to the nters, using coating and /e does not area will be /s at 73.5 50 lbf (680 >lied by any a system of (spring bal- # D 3730 ance). To prevent injury should the dowel come loose, provide a suitable guard by placing over the dowel a length of pipe having a cap at one end and a drilled hole in the cap through which to apply the force. Failure is defined as removal of at least one of the three dowels due to separation between the test panel and the top or glaze coat(s). If failure occurs between the adhesive and the coating, test an addi tional dowel. 10.2.2 If the above portion of test is passed, place the test panel coated side up in a pan containing water maintained at 73.5 3.5F (23 2C). Keep about 0.5 in. (13 mm) of water in contact with the uncoated portion of the panel. At the end of 7 days, pull three more dowels, using a force of 20 lbf (90 N). Dry the coating for 24 h and pull three more dowels, using a force of 30 lbf (135 N). 10.3 Chemical Resistance--An important property of a HIPAC system is its ability to resist spotting, softening, or removal when subjected to household chemicals or strong cleaners. There is no applicable ASTM or Federal test method specifically designated for measuring resistance of HIPAC systems to chemical and cleaning agents, but Test Method D 1308 has been modified as follows: Prepare 5 weight % solutions of sodium hydroxide, sodium hypo chlorite, detergent, hydrochloric acid, sodium phosphate, and sulfuric acid. For each solution saturate a small piece of absorbent cotton, place them on the cured surface, and cover with a 25-mm watchglass. After 4 h, remove, blot dry, allow to recover for 24 h, and examine the exposed surface of the coating for evidence of softening or wrinkling. 10.4 Coating Thickness--Measure total dry film thick ness from the top of the substrate to the top of the applied coating system. When applied to steel, use Test Methods D 1186. When applied to nonmagnetic surfaces, use Test Methods D 1005 if the surface is plain and rigid. 10.5 Flame Spread Test--For some uses HIPAC coatings should not increase fire hazard. Where required, determine the flame spread and smoke development rating in accord ance with Test Method E 84. 10.6 Fungus Resistance--Since HIPAC coatings may be used in food processing plants and locations of high hu midity, they should be resistant to mold growth on the surface. For this test, an environmental chamber is needed. Determine the resistance to mold growth in accordance with Test Method D 3273. 10.7 Heat and Cold Resistance--Buildings can undergo cycling of temperatures that could, through differential thermal expansion between the coating and the masonry substrate, cause failure. There is no applicable ASTM or Federal test methods specifically designated for measuring resistance of HIPAC systems to cold and heat cycles but Test Method D 1211 has been modified as follows: 10.7,1 Place coated panels of the substrate of interest in a cold chamber maintained at 5F (-21C) for 1 h. Remove and immediately place in an oven maintained at 120F (49C) for 1 h. Repeat this cycle 10 times and examine the coating for cracks, checks, or other defects. 10.8 Heat and Humidity Resistance--HIPAC coatings can be subjected to environmental conditions where high heat and humidity are present. There is no applicable ASTM or Federal test method specifically designated for measuring resistance of HIPAC systems to heat and humidity but Practice D 2247 has been modified as follows: 10.8.1 Coat panels with the complete system and expose to an environment of 95 % relative humidity minimum, and I40F (60"C) for 7 days in an enclosed cabinet. Determine the 60-deg gloss before and after by Test Method D 523 and color change by Method D 2244. 10.9 Impact Resistance--An important property of HIPAC coatings is their ability to withstand impact when objects are accidentally knocked against them. Determine impact resistance in accordance with Test Method D 2794, except use zinc phosphate-treated steel panels. Some mate rials, such as urethanes, require a wash primer or an epoxy primer to give the adhesion needed for this test. Apply top or glaze coat(s) at a minimum dry-film thickness of 3 mils (75 mm) and examine the surface of the impacted coated area under 7x magnification for cracking and crazing of the coating immediately after testing and 72 h after the test. 10.10 Perspiration Resistance--HIPAC coatings can sometimes come in contact with perspiration that could stain the coating. There are no ASTM or Federal test methods to measure perspiration resistance of HIPAC systems but where considered important the following method can be used: 10.10.1 Prepare synthetic perspiration fluid having the following composition by weight: Urea J2( ( 3 Na2SO4-I0H2O NaCl Acetic acid (5 % solution) ' 2o Anhydrous lanolin 1.30 0.11 0.65 2.71 1.08 10.85 83.30 10.10.1.1 Dissolve the urea and inorganic salts in the acetic acid solution and water. Heat the lanolin to 45C and add the solution to form an emulsion. Combine with a dye and wetting agent in the following proportions: Scarlet red Methanol Wetting agent Synthetic perspirant 0.1 3.7 3.8 92.4 10.10.1.2 Dissolve the dye in the methanol, then mix with the wetting agent and synthetic perspirant. Apply an excess ofthe mixture to a small area of a test panel, using a 1 in. (25 mm) wide artist's brush. Cover with a 25-mm watchglass and place the panel in an oven at 120 3.5F (49 2C), for 4 h. Remove the panel and allow to cool at room temperature for 1 h. Wipe off the excess with a soft dry cloth. If the stain is not completely removed, subject the panel to not more than 25 cycles of the washing procedure described in Method 6141 of Federal Test Method Standard No. 141. Examine the film under 7x magnification for stain retention. 10.11 Scrubbability--The ability of an interior finish to resist scrubbing is an important property. The referenced method provides a measure of the wet abrasion resistance of a film. However, wet abrasion resistance is not necessarily a measure of how well soils or stains can be removed since some porous materials have good scrubbability but poor stain cleansability. Test the coating for at least 4000 cycles in accordance with Method 6142 of Federal Test Method Standard No. 141 except use smooth cement asbestos board complying with Specification C 220 as substrate. Apply the coating system to be tested in conformance with the manu facturer's printed directions for surface preparation, mixing, 563 DUPO 502 97744 * D 3730 Desi application, coverage, and curing time (usually 21 days) at standard conditions of temperature and humidity. tions for the time specified by the manufacturer but,, more than 21 days. 5ot 10.12 Cleansability--The ability to remove marks satis 10.12.2 Stain Application--Typical household stain m factorily without damaging the film is an important property dia are coffee, grape juice, ink, soil, crayon, and lipstick. (? of interior finishes, A test method to determine how well Practice D 3023 for specific materials.) Applythe stain toe? stain and soils can be removed from a cured film is now in about 1 in. (25 mm) apart in the center of die panel. ApJ5 preparation and will be included in the guides when it is crayon and lipstick by normal hand pressure; smear coffj approved by ASTM. Test methods used by the paint industry grape juice, and ink with an artist's brush; apply soil un(j ' consist of applying various household soils or stains to the load by placing a 1-lb (500-g) weight on top of an applicate cured film and attempting to remove them by a washing or in such a manner that the soil is uniform in thickness. ' scrubbing operation. A suggested test for washability, based 10.12.3 Removal ofStain--After allowing the stains to ^ on Method 6141 of Federal Test Method Standard No. 141 for 24 h under standard conditions, wash the stains for <{ K is given below: cycles in accordance with Method 6141 of Federal fe$t Scope 10.12.1 Coating Application--Coat a test panel approxi mately 12 by 4 in. (305 by 102 mm) with the complete system of the product under test, applying the glaze or top Method Standard No. 141. Observe the panel for stai5 removal during and at the end of 100 cycles. If a stain jj removed in 100 cycles or less, report the number of cycles 1.1 This f olet energy. coating to at least 3-mils (75-mm) dry-film thickness is not more than two coats. Allow to cure under standard condi required. If not removed in 100 cycles, report the test as a failure. 2 Referenct j 2.1 ASTh The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. >658 Te ; Coating I p968 Te This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are invited eitherforrevision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. * Coating p1474 T Coating D2197T l Scrape D2336 I Throug Wood D2793 ` Coatin D 27941 the Eft D 3023 I tory-A Reage: D3281 ' Coati' D3359 Test2 D3363 3. Termin 3.1 Des 3.1.1 ci the final s to end-use and purcb \ 3.1.2 u. applicatio mechanist S; equipmen 1 This pra Related Coal 001.55 on F Current e 564 DUP0502 97745 3732 - 82 (Reapproved 1S89)e1 "ain tick. 'n m el-Ai ir Coi ail ur ins S fo 2ral for Standard Practice for Reporting Cure Times of Ultraviolet-Cured Coatings1 This standard is issued under the fixed designation D 3732; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1 NLM' --Editorial changes were made throughout in April 1989. . ScPe I [ This practice applies to all coatings cured by ultravi olet energy- i Referenced Documents II ASTM Standards: p658 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive2 p968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive2 p 1474 Test Methods for Indentation Hardness of Organic Coatings2 02197 Test Methods for Adhesion of Organic Coatings by Scrape Adhesion2 2336 Practice for Specifying Properties from Liquid Through Cured State for Coatings Factory Applied to Wood Products2 >2793 Test Method for Block Resistance or Organic Coatings on Wood Substrates2 D 2794 Test Method for Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact)2 D 3023 Practice for Determination of Resistance of Fac tory-Applied Coatings on Wood Products to Stains and Reagents2 D 3281 Test Method for Formability of Attached Organic Coatings with Impact-Wedge Bend Apparatus2 D3359 Test Methods for Measuring Adhesion by Tape Test2 D 3363 Test Method for Film Hardness by Pencil Test2 1. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 cure--the condition of a coating after conversion to the final state of cure as measured by tests generally related to end-use performance and mutually agreeable to supplier ami purchaser. 3.1.2 ultraviolet curing--conversion of a coating from its application state to its final use state by means of a mechanism initiated by ultraviolet radiation generated by equipment designed for that purpose. 4. Significance and Use 4.1 This practice provides a guide whereby all pertinent variables relating to the ultraviolet cure of a coating are described. 5. Procedure. 5.1 Apply the coating to be cured to the desired substrate at a film thickness typical to that normally used. After approximately the time delay encountered in production pass the coated substrate through the curing equipment and subsequently test for cure, as defined in 3.1.1, using the appropriate methods listed in 5.1.1 through 5.1.11. The most commonly used test methods are listed in 5.1.1 through 5.1.4. 5.1.1 Impact Resistance--Test Method D 2794. 5.1.2 Film Hardness--Test Method D 3363. 5.1.3 Solvent Rub Test--Hold a pad of cheesecloth or other cloth saturated with an agreed-upon solvent, usually methyl ethyl ketone, over two adjacent fingers using a protective covering. Rub the wet pad back and forth across a 100-mm portion of the cured film using vigorous pressure, one forward and one backward movement constituting one double mb. Take the end point as the number of double mbs required to soften or penetrate the film. Fully cured films are normally required to resist a specified number of mbs and the result of the test is given as exceeding the limit or failing the test. 5.1.4 Sandability--Ultraviolet cured fillers are usually judged by their sandability with an agreed-upon grit of paper. This test is often made immediately after the material leaves the ultraviolet processor. 5.1.5 Specifying Properties--Practice D 2336. 5.1.6 Abrasion Resistance--Test Methods D 658 and D968. 5.1.7 Indentation Hardness--Test Methods D 1474. 5.1.8 Adhesion--Test Methods D 2197 and D 3359. 5.1.9 Block Resistance--Test Method D 2793. 5.1.10 Formability--Test Method D 3281. 5.1.11 Stain and Reagent Resistance--Practice D 3023. 5.2 Repeat the application, curing, and testing with fresh material on fresh substrates until the shortest time that yields a cured film is obtained. 1 This practice is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee Wl.55 on Factory-Applied Coatings on Preformed Products. Current edition approved Oct. 29, 1982. Published January 1983. Originally Published as D 3732 - 78. Last previous edition D 3732 - 78. 2 Annual Book ofASTM Standards, Vol 06.01. 6. Report 6.1 Ultraviolet curing equipment is available with several design variables. Therefore, include the following informa tion with results where applicable: 6.1.1 Number of bulbs, 565 i j DUP050297746 # D 3732 6.1.2 Bulb type (intensity, spectral distribution, composi tion), 6.1.3 Bulb age, 6.1.4 Bulb location (height from work and orientation to workpiece), 6.1.5 Reflector design, 6.1.6 Conveyor speed or exposure time to achieve cure, 6.1.7 Substrate, 6.1.8 Coating identification and age of sample if known. 6. i .9 Wet film thickness, 6.1.10 Temperature conditions in the curing unit, 6.1.11 Curing environment (air, nitrogen, or other phere), 6.1.12 Cure tests used (refer to Section 5), and 6.1.13 Age of cured film when tests were run. 7. Keywords 7.1 cure time; ultraviolet-cured coatings The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. r 2. Refer 2.1 A D UD 13< (Fi E 18' M ici 3. Sui 3.1 dardi formcolui wate detei duci 4. S 4. (VC wat vid< cor. and mil put DUP050297747 Designation: D 3792 - 91 unit, 0Ther^ id Standard Test Method for Water Content of Water-Reducible Paints by Direct Injection Into a Gas Chromatograph1 This standard is issued under the fixed designation D3792; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of iast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapprovai. j. Scope 1.1 This test method is for the determination of the total water content of water-reducible paints. It has been evalu ated for latex systems (styrene-butadiene, poly(vinylacetate)acrylic, acrylic). It has not yet been evaluated for other water-reducible paints but is believed to be applicable. The established working range of this method is from 40 to 55 % water. There is no reason to believe that it will not work outside of this range. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water2 D1364 Test Method for Water in Volatile Solvents (Fischer Reagent Titration Method)3 E 180 Practice for Determining Precision Data of ASTM Methods for Analysis and Testing of Industrial Chem icals4 3. Summary of Test Method 3.1 A suitable aliquot of whole paint is internally stan dardized with anhydrous 2-propanol, diluted with dimethylformamide, and then injected into a gas chromatographic column containing a porous polymer packing that separates water from other volatile components. The water content is determined from area calculations of the materials pro ducing peaks on the chromatogram. 4. Significance and Use 4.1 With the need to calculate volatile organic content (VOC) of water-reducible paints, it is necessary to know the water content. This gas chromatographic test method pro vides a relatively simple and direct way to determine water content. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved May 15, 1991. Published July 1991. Originally published as D 3792 - 79. Last previous edition D 3792 - 86. 2 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 3Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 15.05. TABLE 1 Instrument Conditions Detector Temperatures, C: Sample inlet Detector Column'1 initial Final - Program rate Carrier Gas Flow rate, mljmin Detector current Specimen size thermal conductivity 200 240 80 170 30/min helium or nitrogen 50 150 mA IpL *For isothermal operation set the column temperature at 140*C. After the 2-propanol has cleared the column adjust the temperature to 170C until DMF clears the column. Reset the temperature to 140C for subsequent runs. 5. Apparatus 5.1 Gas Chromatograph--Any gas-liquid chromato graphic instrument having a thermoconductivity detector may be used. Temperature programming capability is pref erable, but isothermal operations may be adequate. See Table 1. 5.2 Column--The column should be 4 ft (1.22 m) of Vis-in. (3.2-mm) outside diameter tubing of stainless steel, or other suitable material, packed with 60/80 mesh (180 to 250 pm) porous polymer packing material.5 A replaceable glass sleeve, glass wool plug, or other suitable material may be placed on the entrance end of the column to retain any nonvolatile materials. This will minimize sludge buildup in the column. 5.3 Recorder--A recording potentiometer with a full-scale deflection of 1 to 10 mV, full-scale response time of 2 s or less and sufficient sensitivity and stability to meet the requirements of 5.1. 5.4 Liquid Charging Devices--Micro syringes of 10 or 25-fiL capacity. 6. Column Conditioning 6.1 Procedure--The packed column is installed in the gas chromatographic unit leaving the exit end disconnected from the detector. This will prevent any contamination of the detector with the column bleed. Set the helium or nitrogen flow rate at 20 to 30 mL/min if a Vi-in. (3.2-mm) outside diameter column is used. Purge the column 5 or 10 min before heating. Heat the column from room temperature to 200C at 5C/min and hold this temperature for at least 12 h (overnight). At the end of this time, heat the column at 5 Parapak Q, a trademark of Waters Assoc., Inc., Milford, MA, has been found satisfactory. Any other porous polymer packing or other column giving equivalents or superior performance may be used. These products are available from most gas chromatograph suppliers and distributors. 567 DUP050297748 <) D 3792 5C/min to 250C (the maximum temperature for this packing) and hold for several hours. Cool the column to room temperature and connect the column detector. Reheat the column to 250C at 5"C/min to observe if there is column bleed. Optimum conditioning of this column may take several cycles of the heating program before a good recorder baseline is achieved. 6.2 Before each calibration and series of determinations (or daily) condition the column at 200C for 1 h with carrier gas flow. 7. Reagents and Materials 7.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 7.2 Purity of Water--Unless otherwise indicated, refer ence to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 7.3 Carrier Gas--Helium of 99.995 % or higher purity. High-purity nitrogen may also be used. NNO' I--Care should be taken that any moisture that may be present in the carrier gas is eliminated through the use of a suitable carrier gas purifier. Trace levels of water will accujjiulate on the column at low oven temperatures and may affect the reproducibility as well as the accuracy of the determination. 7.4 Dimethylformamide (DMF) (Anhydrous) gas chroma tography, spectrophotometric quality (Note 2). 7.5 2-Propanol (Anhydrous) (Isopropanol)--See Note 2. 7.6 Septum Sample Vials, 10-mL capacity with fluorocar bon-faced septa are preferred. NPQ' 2--Determine the water content of the DMF and 2-propanol by Karl Fischer titration in accordance with Test Method D 1364. Dry the 2-propanoi if water is found in it or replace with anhydrous grade. 8. Hazards 8.1 Dimethylformamide is hazardous. Check the suppli er's Material Safety Data Sheet (MSDS) before use. 9. Preparation of Apparatus 9.1 Install the column in the chromatograph and establish the operating conditions required to give the desired separa tion (see Table 1). Allow sufficient time for the instrument to reach equilibrium as indicated by a stable base line. Control the detector temperature so that it is constant to within 1C without thermostat cycling which causes an uneven baseline. Adjust the carrier-gas flow to a constant value. 10. Calibration 10.1 Using the information in Table 1 (as a guide), select the conditions of temperature and carrier gas flow that give the necessary resolution of the components. .prate of 10.2 drous Determination 2-propanol is uosfeRdelaastivaenReinspteornnsael Fsatcatnodrasr-d;,Anvhv 10.2-4.1 ,foPano1 ? response factor to water relative to the standard is :t L area of mined by means of the following procedure. See Fig. i f ^ tV2.4.2 typical chromatogram. It is good practice to determine eans of t relative retention time daily or with each series of determ' nations. ^ 10.2.1 Weigh about 0.2 g of water and 0.2 g of 2-propa,,r, to 0.1 mg into a septum sample vial. If it has W ^Jiere: _ determined that a correction for the water content necessary, weigh 2 mL of dimethylformamide (DMF) jJ V the vial. If the DMF is anhydrous, simply add 2 mL of it weighing is not necessary. 4i I _ " 10.2.2 Inject a 1-p.L aliquot of the above solution into tie 4' ,o _ column and record the chromatogram. The retention oi 3 and approximate retention times after the air peak are (h water, about 0.7 min; (2) 2-propanol, about 2.8 min; and (h DMF, about 7 min. 10.2.3 The preferred procedure to obtain the water con. tent of the DMF is the Karl Fischer titration (Note 1). If thjj has been determined, calculate the response factor for water lj. Proe 11.1 V Note 3) 2-mL of containi' by means of the following equation: WA HaO {WHiQ + PW,)A,. NRS' peaks. Co 11.2 suitable where: R = response factor, W: = weight of 2-propanol, w,HjO = weight of water added, W, = weight of dimethylformamide, ^HjO = area of water peak, A, = area of 2-propanol peak, and P = weight % water in DMF 100 allow th ; the chr I used. 11.3 prepare Record Table 12. Ct 10.2.4 If Karl Fischer titration is not available, the fol lowing procedure may be used to obtain a reasonable 12.1 propai the ar on a recon How< and t 12 meat wher ^H.C V W, W,, 6 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY and the "United States Pharmacopeia." 568 DUP0502 97749 # D 3792 estimate of the response factor: 10.2.4.1 Inject the same size aliquot of DMF and 2- propanol mixture, but without added water, as a blank. Note tlie area of the water peak in the blank. 10.2.4.2 The response factor for water is calculated by ,,ieans of the following equation: ,, W(AH,o ~ S) where: H = response factor, If. = weight of 2-propanol, ffH o = weight of the water, g. 1 = area of 2-propanol peak, gn0 = area of the water peak, and g 1 = area of the water peak in the blank. jl. Procedure 11.1 Weigh to 0.1 mg, 0.6 g of water-reducible paint (see Mote 3) and 0.2 g of 2-propanol into a septum vial. Add 2-mL of DMF into the vial. Seal the vial. Prepare a blank containing the 2-propanol and DMF but no paint. NTU' 3--Check each paint system to be analyzed for interfering peaks. Coalescing agents do not interfere with this determination. 11.2 Shake the vials on a wrist action shaker or other suitable device for 15 min. To facilitate settling of solids allow the vials to stand for 5 min just prior to injection into the chromatograph. Low-speed centrifugation may also be used. 11.3 Inject a 1-pL sample of the supernatant from the prepared solutions into the chromatographic column. Record the chromatograms using the conditions described in Table 1. 12. Calculations 12.1 Measure the area of the water peak and the 2propanol internal standard peak and multiply each area by the appropriate attenuation factor to express the peak areas on a common basis. Use of an electronic integrator is recommended to obtain the best accuracy and precision. However, triangulation, planimeter, paper cut out, or ball and disk integrator may be used. 12.2 Calculate the water concentration in the paint by means of the following equation: A, xWpxR where: 4' ,o -- urea of water peak, A, = area of 2-propanol peak, Wt = weight of 2-propanol added, Wp = weight of paint, and R = response factor determined in 10.2. 12.3 Correction for Water Content ofSolvent: 12.3.1 If the blank indicates the presence of a detectable peak for water in the dimethylformamide used as solvent, make a correction in the calculation. 12.3.2 The water content of the dimethylformamide de termined by either chromatography (10.2.4) or, preferably, Karl Fischer titration (10.2.3) is used to make the correction. Calculate the water content due to the solvent by using the following equation: H20(S),%=TM^ WP where: Ws = weight of dimethylformamide, Wp = weight of paint, and P ~ weight % water in DMF 100 12.3.3 The water content of the paint in this case is the difference between the total percent determined in 12.2 and the correction for the solvent water content as determined in 12.3.2. 13. Precision and Bias7 13.1 The precision estimates are based on an inter laboratory study in which nine different laboratories ana lyzed in duplicate on two days four samples of waterreducible paints containing from 40 to 55 % HzO (theoretical). The results obtained were analyzed statistically in accordance with Practice E 180. The within-laboratory coefficient of variation was found to be 1.0 % relative at 34 df and the between-laboratories coefficient of variation 2.6 % relative at 30 df. Based on these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level. 13.1.1 Repeatability--Two results, each the mean of du plicate deteminations, obtained by the same operator on different days should be considered suspect if they differ by more than 2.9 % relative. 13.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 7.5 % relative. 13.2 Bias--Bias has not been determined. 14. Keywords 14.1 gas chromatograph; water content of paints by gas chromatograph 7 Supporting data are available from ASTM Headquarters. Request RR: DO 1 1022. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 569 DU PO50297750 Designation: D 3793 - 89 Standard Test Method for Low-Temperature Coalescence of Latex Paint Films1 This standard is issued under the fixed designation D 3793; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval, A superscript epsilon (f) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the comparative coalescence of a series of latex paints by determining the porosity of films dried at standard and at low temperature. Porosity is evaluated with a penetrating medium as in Test Method D 3258. 1.2 The texture of the film, which can affect cleanup, will influence the results of the test. Stain applied to a high-hiding paint will not lower the reflectance as much as the same stain applied to a low-hiding paint of equal porosity. These points must be considered in comparing the different paints. 1.3 This method should be used only for comparative testing within one laboratory, as the numerical results obtained by different laboratories do not usually agree. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D3258 Test Method for Porosity of Paint Films2 E 97 Test Method for Directional Reflectance Factor, 45-deg O-deg, of Opaque Specimens by Broad-Band Filter Reflectometry3 3. Summary of Test Method 3.1 The test paints are applied to porous cardboard panels, dried at standard temperature and at 40F (4.5C) with 50 % relative humidity in both cases, and their re flectances measured. A special colored penetrating medium is applied to each, the excess removed in a specified manner, and reflectances measured again. The difference between the readings on the stained and unstained films indicates the porosity of that film; the difference between the readings for the two temperatures indicates the coalescence of that film compared to others in the series. 4. Significance and Use 4.1 This test method provides no absolute information, rather ranking only of the selected series of paints. 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee EX) 1.42 on Architectural Finishes. Current edition approved March 31, 1989. Published May 1989. Originally published as D 3793 - 79. Last previous edition D 3793 - 84. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 4.2 This test method can provide a pass-fail situation known acceptable and unacceptable paints are included in the test. n 5. Apparatus and Materials 5.1 Plate Glass Panel (base for cardboard panel). 5.2 Strippable Adhesive.4 5.3 Test Panel--Smooth porous cardboard panel such as the back of a white drawdown chart.5 5.4 Film Applicator, 6 in. (150 mm) wide with a clearance of 6 mils (150 pm).6 5.5 Film Applicator, 5Vi in. (140 mm) wide with a clearance of 10 mils (255 pm).7 8 5.6 Reflectometer, meeting the requirements of Test Method E 97. NVW' --Although Test Method E 97 specifies a 45/0 reflectometer, other types of instruments that measure the Y tristimulus value caa be used. 5.7 Cold Cabinet, maintaining 40 2"F (4.5 l`C) and 50 dfc 5 % relative humidity. 5.8 Camel's Hair Brush, approximately Vi in. (13 mm) wide. 5.9 Plastic Wash Bottle, about 16 oz or 500 mL con taining mineral spirits of the odorless type. 5.10 Penetrating Medium8--A proprietary composition of pigments or dye, or both, dispersed in a liquid vehicle. 5.11 Filter Paper. 6. Procedure 6.1 Adhere a porous cardboard test panel to each of as many plate glass panels as needed, using the strippable adhesive and ensuring that the cardboard panels are smooth with no wrinkles. 6.2 For each paint, coat one panel using the 6-mil (150-pm) clearance drawdown blade. Air dry 48 h under 4 Any strippable adhesive such as represented by the following formulas: Vinyl acrylic emulsion such as Flexbond 325, available from Air Products and Chemi cals, P.O. Box 538, Allentown, PA 18105 (800 parts by weight) or polyethylene glycol, molecular weight 1500, such as Carbowax 1500, available from Union Carbide Corp., 1300 Lakeside Ave., Cleveland, Ohio 44114 (16 parts by weight). 5 Form WA or equivalent white cardboard drawdown chart available from the Leneta Co., P.O. Box 576,'Ho-Ho-Kus, N3 07423, has been found satisfactory for this purpose. 6 Bird film applicators or their equivalent available from Byk-Gardner, Inc., Gardner Laboratory, 1110 East West Highway, Silver Spring, MD 20910, have been found satisfactory for this purpose. It should be noted that some applicators are marked with the nominal wet film thickness which is one halfof the clearance. 7 The Dow latex film caster available from Byk-Gardner, Inc. has been found satisfactory ijor this purpose. 8 K & N S-68 Special Compound available from: K &. N Laboratories, Inc. 5331 Dansher Rd., Countryside, IL 60525, has been found suitable for this purpose. aa^arc!c %VDet 5sSmt. lanel wlt trating m as ab0VC tnedium. medium minera! t fenioved wash bo down ac forms at confirms is esseni remains 6.6 F h. As be on the i them. 6.7 I clearan cold ca ,5 % rel 6.8 thorou: one pa process 570 DU P050297751 ituation if lduded in l). lei such as a clearance de with a s of Test eflectometer, value can be t TC) and i. (13 mm) } mL conomposition . vehicle. ach of as strippable re smooth the 6-mil +8 h under i D 3793 ndard conditions of 73.5 3.5F (23 2"C) and 50 5 % slttive humidity. ^3 Determine the percent reflectance (Y tristimulus ,ue) of the dry films. Use the green filter when using a hectometer. When making these readings, back up each with a flat rigid opaque object and mark the area on SjjCh the reading was made. *6.4 Using the 10-mil (255-pm) blade, apply the pene- ,ting medium to each test paint, covering the area marked V above and drawing the applicator blade in the same Erection as before. 6.5 After 5 min 15 s, wash off excess penetrating Jium. To do this hold the panel vertically and remove the medium using the camel's hair brush wet with odorless mineral spirits. Repeat the process until most of the excess is removed then apply the mineral spirits directly from the waSh bottle to the area above the stain and allow to flow rjown across the stained area. Pause to observe the bead that forms at the bottom of the panel. If the bead is not clear, continue washing with odorless mineral spirits until the bead is essentially clear. Test with filter paper to be sure no dye remains in the bead. 6.6 Hang the panel in a vertical position and air dry for 3 h. As before, read the percent reflectance over the same area on the panels with the same flat rigid opaque object behind them. 6.7 Place one panel for each paint, the 6-mil (150-p.m) clearance drawdown blade, and the can of each paint into the cold cabinet maintained at 40 2F (4.5 1C) and 50 5 % relative humidity. 6.8 At the end of 24 h remove one can of paint and stir thoroughly. Then remove the drawdown blade along with one panel and make the drawdown immediately. Repeat the process for each paint under test. All items should be kept out of the cold cabinet only long enough to make draw downs. ^'P Place all the panels back into the cold cabinet and dry for 48 h. 6.10 Repeat the reflectance readings before and after application of the penetrating medium to these panels in accordance with 6.3, 6.4, 6.5, and 6.6. 7. Calculation 7.1 For each paint calculate the difference between the percent reflectance of the unstained and stained films at both standard and low temperatures. These two differences indi cate the porosity of the film formed at the two temperatures. Calculate the low-temperature coalescence of each paint as the ratio of the porosity at low temperature to the porosity at standard temperature which is indicative of relative coales cence. 8. Report 8.1 Report the order of low-temperature coalescence of the test paints in the series. 9. Precision and Bias 9.1 In an interlaboratory study of this test method in which one operator in each of six laboratories tested paint films of three normally different levels of coalescence, all six laboratories ranked the three paints in the same order of coalescence. However, there were considerable differences between the values obtained by the laboratories for any one paint. 10. Keywords 10.1 coalescence; latex paint; porosity The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. formulas: Vinyl icts and Chemior polyethylene tie from Union arts by weight), ailable from the i satisfactory for k-Gardner, Inc., ID 20910, have lome applicators of the clearance, has been found aboratories, Inc. suitable for this DUP0502 97752 Designation: D 3794 - 791 An American Standard Practice for Testing Coil Coatings1 This standard is issued under the fixed designation D 3794; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. (1 NXY' --Table 1 was editorially corrected in April 1987. 1. Scope 1.1 This practice covers procedures for testing coil coat ings. The test methods included are listed in Table 1. Where more than one test method is listed for the same character istic, no attempt is made to indicate superiority of one method over another. Selection of methods to be followed must be governed by the requirements in each individual case, together with agreement between the producer and user. 1.2 This practice also refers to methods developed specif ically for the Coil Industry by the National Coil Coaters Association.12 2. Referenced Documents 2.1 ASTM Standards: B 117 Method of Salt Spray (Fog) Testing2 B 287 Method of Acetic Acid-Salt Spray (Fog) Testing3 D522 Test Methods for Mandrel Bend Test of Attached Organic Coatings4 D523 Test Method for Specular Gloss4 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces4 D 659 Test Method for Evaluating Degree of Chalking of Exterior Paints4 D 660 Test Method for Evaluating Degree of Checking of Exterior Paints4 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints4 D714 Test Method for Evaluating Degree of Blistering of Paints4 D 822 Practice for Conducting Tests on Paint and Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light- and Water-Exposure Apparatus4 D 870 Practice for Testing Water Resistance of Coatings Using Water Immersion4 D 1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers4 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base4 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DOL.53 on Factory-Precoated Strip Metal. Current edition approved May 25, 1979. Published October 1979. 2 Annual Book ofASTM Standards, Vols 03.02 and 06.01. 3 Discontinued; see 1988 Annual Book ASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vol 06.01. D1200 Test Method for Viscosity by Ford Viscosity q D 1210 Test Method for Fineness of Dispersion of ment-Vehicle Systems4 D 1212 Methods for Measurement of Wet Film Thick of Organic Coatings4 D1308 Test Method for Effect of Household Cherniy on Clear and Pigmented Organic Finishes4 D1353 Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and f>j. lated Products3 D 1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap. plied to a Nonferrous Metal Base4 D1474 Test Methods for Indentation Hardness ofOrganic Coatings4 D1654 Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive Environments4 D1729 Practice for Visual Evaluation of Color Differences of Opaque Materials6 D2092 Practices for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Painting4 D2196 Test Methods for Rheological Properties of NonNewtonian Materials by Rotational (Brookfield) Vis cometer4 D 2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates4 D2247 Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity4 D2248 Practice for Detergent Resistance of Organic Finishes4 D 2454 Practice for Determining the Effect of Overbaking on Organic Coatings4 D2697 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings4 D 2794 Test Method for Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact)4 D 2803 Test Method for Filiform Corrosion Resistance of Organic Coatings on Metal4 D 3003 Test Method for Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates4 D3281 Test Method for Formability of Attached Organic Coatings with Impact-Wedge Bend Apparatus4 D3359 Test Methods for Measuring Adhesion by Tape Test4 5 Annual Book ofASTM Standards, Vol 06.03. 6 Annual Book ofASTM Standards, Vol 14.02. 572 DUP0502 97753 D 3794 xity cU04 ,nf% Thj<*rw "beinicais 1 vlatile and rfnient 0f t]ngs Ap. ,f Organic r Coated its4 inferences 1 (Galva- of Noneld) Vis- Terences es4 boatings Organic TABLE 1 List of Test Methods and Recommended Practices Section ASTM Method Liquid Paint Properties: Viscosity: Rotational viscometer Ford cup Zahn cup Weigtit solids Volume solids Fineness of dispersion pH Metal Treatment Treatment for zinc-coated steel Phosphate weight on steel Phosphate weight on hot-dipped galvanized Chromate weight on aluminum Panel Preparation: Drawdowns Wet film thickness Sake schedule Physical Properties of Cured Coating: Dry film thickness: Nonmagnetic base Magnetic base Micrometre (destructive) Color difference Gloss Hardness: Pencil hardness Indentation hardness Flexibility: Impact Wedge bend Conical mandrel T bends Adhesion (tape) Pressure marking and blocking Overbake Detergent resistance Stain resistance Exterior and Accelerated Durability Tests: Outdoor exposure Accelerated durability: Salt spray Acidified salt spray Humidity Water immersion Accelerated weathering Accelerated weathering Filiform corrosion 6 6.1 6.1.2 6.1.2 6.1.3 6.2 6.3 6.4 6.5 7 7.2 7.3.1 7.3.1 7.3.2 3 8.5 8.6 8.7 9.0 9.1 9.1 9.1.1 9.1 9.2 9.3 9.4 9.4.1 9.4.2 9.5 9.5.2 9.5.3 9.5.4 9.5.5 9.6 9.7 9.8 9.9 9.10 10 10.1 10.2 10.2.1 10.22 10.2.3 10.2.4 10.2.5 10.2.5 10.2.6 D2196T D1200 D1353 D2697 01210 E70 D2092 D1212 D1400 D1186 D1005 D 2244 4 D1729 D523 D 3363 D1474 D2794 D3281 . D522 D3359 D3003 D2454 D2248 D1308 D1014 B117 B287 D2247 D870 822 D3381 D2803 t Editorially coirected. NCCA Method NCCA 11-1 NCCA 11-3 NCCA 11-2 -rbaking latter in atings to tance of | 31ocking rates4 Organic ; , ->y Tape I D 3361 Practice for Operating Light- and Water-Exposure Apparatus (Unfiltered Open Flame Carbon-Arc Type) for Testing Paint, Varnish, Lacquer, and Related Prod ucts Using the Dew Cycle4 D3363 Test Method for Film Hardness by Pencil Test4. E 70 Test Method for pH of Aqueous Solutions with, the Glass Electrode7 8 2.2 National Coil Coalers Standards. s No. II-1, Specification for Determination of Phosphate Coating Weights on Steel No. II-2, Specification for Coating Weight Determination for Chromate Conversion Coatings on Aged or Baked Aluminum Alloy Panels 7 Annual Book ofASTAf Standards, Vol 15.05. 8 Copies of National Coil Coalers Assn, methods are available through NCCA Headquarters, 1900 Arch St., Philadelphia, PA 19103. No. II-3, Specification for Determination of Phosphate Coating Weight on Hot Dip Galvanized and Electrogalvanized Steel 3. General Requirements 3-1 All tests shall be made in diffused light (not direct sunlight) and at 73.5 3.5F (23 2C) and 50 5 % relative humidity, immediately after baking unless otherwise specified; 4. Definitions 4.1 coil coating--application of coatings or films to con tinuous metal coil stock. 4.2 metal pretreatment--chemical treatment normally ap plied to the metal substrate prior to prime or finish coating. The treatment is designed to react with and modify the metal substrate to produce a surface suitable for coating or adhe sive bonding. 573 DUPO 50297754 # D 3794 4.3 reverse roller coat--coating with the applicator or coating roll revolving in a direction opposite to that of the strip. 4.4 direct roller coat--coating with the applicator or coating roll revolving in the same direction as the strip. 5. Sampling 5.1 The number of samples per unit of production shall be agreed upon between producer and user. 6. Liquid Coatings Properties 6.1 Viscosity: 6.1.1 Coatings in the coil industry cover a wide range of generic qualities with many of them having non-Newtonian characteristics. It is therefore important to consider the behavior of these coatings under different shear conditions as well as measuring efflux viscosity by the Ford cup. 6.1.2 Determine viscosity in accordance with Test Methods D 2196 and D 1200. 6.1.3 Viscosity by Zahn cup.9 6.1.3.1 Apparatus--Standard Zahn cup with specified orifice, a No. 4 or 2 orifice is most commonly used. Stop watch. 6.1.3.2 Procedure--Clean the Zahn cup thoroughly. The sample must have a volume of at least 1 pt and the Zahn cup and sample must be 73.5 3.5F (23 2C). Thoroughly mix the sample. Dip the Zahn cup in a vertical position into the sample being tested, making certain the cup is completely immersed in the liquid but do not allow the cup to touch the bottom of the container. Rapidly lift the cup out of the sample and as the top edge of the Zahn cup breaks the surface start the stop watch. Stop the watch when the first break in the flowing stream of liquid is noted at the orifice exit. Record the seconds elapsed, temperature and number of the Zahn cup used. 6.2 Weight Solids (NVM)--Determine nonvolatile matter in accordance with Test Method D 1353. 6.3 Volume Solids--Determine volume solids in accor dance with Test Method D 2697. 6.4 Fineness of Dispersion--Determine fineness of grind in accordance with Test Method D 1210. 6.5 pH: 6.5.1 Control of pH in the pretreatment section of the coil line as well as of waterborne coatings is important in production. 6.5.2 Determine pH in accordance with Method E70. 7. Metal Pretreatment (Conversion Coating) 7.1 The successful performance of any coil-coated mate rial is dependent not only on the organic coating used but also on the metal preparation. Metal preparation in the coil coating industry usually consists of one of the following: (*> Clean (b) Rinse (O Formation of conversion coating (d) Rinse (a) Clean (*) Rinse (ri Formation of conversion coating Drying (e) Posttreatment of conversion coating (/) Drying 7.1.1 The metal pretreatment promotes maximum f ability and improves adhesion and environmental expo^ resistance of the coil coating material. Cleaners, convex coating treatments and posttreatments used vary witw performance desired, the paint and the metal. Because th6 m is an interdependency between the cleaning, couve^ coating, and posttreatment steps, in order to obtain re!ev^ test data, it is necessary that the chemicals, times, conceit? tions, temperatures, and application methods be as close3' possible to those encountered under production condition 7.2 In the case of zinc coated steel surfaces, Piactj D2092 Methods A, B, C, and D illustrate the variety 5. pretreatments available. 7.3 Coating Weight of Metal Pretreatment--In tnam, cases, one quality control measurement is the coating of the metal pretreatment formed. The following method are recommended: 7.3.1 Zinc or Iron Phosphate Conversion Coatings ,,,, Steel--Determine the weight of the iron phosphate convej. sion coating on steel in accordance with NCCA II-1 and tht weight of the phosphate conversion coating on hot dip galvanized steel in accordance with NCCA II-3. 7.3.2 Chromate-Conversion Coatings on Aluminum--]^ termine the weight of the chromate conversion coating on aluminum in accordance with NCCA II-2. 8. Panel Preparation 8.1 Summary ofMethod--This method includes substrate and pretreatment selection for application of coatings by wire wound draw-down bars10 on laboratory panels. 8.2 Choice of Substrate--The substrate to be coated, substrate size, gage, temper, alloy, pretreatment to be used shall be agreed upon between the producer and user. Avoid using treated substrates that have been contaminated by handling or cleaned with solvents or cleaners. 8.3 Degassing of Substrate--Some galvanized substrates tend to absorb gasses on aging. To avoid blistering when the substrate is coated and baked it may be necessary to degas the substrate by heating and cooling to room temperature prior to application ofthe coating. The time and temperature of the degassing cycle shall be agreed upon between the producer and user. 8.4 Drawdowns: 8.4.1 Apparatus--Wire-wound draw-down bars, stainless steel bars preferably '/z in. (12.7 mm) in diameter to prevent bowing during application. The choice of the specific draw down bar is dependent on the dry film thickness required and the volume solids of the coating being tested. 8.4.2 Procedure--Secure the substrate to be coated on a hard uniform, even surface. Place an excess amount of the coating to be used near the top of the substrate. Place the draw-down bar in the puddle of the coating to be applied. Rotate or turn the draw-down bar slightly in the coating puddle to ensure complete distribution of the coating in the 9 Zahn Cups are available from Paul N. Gardner Co. Inc., 316 N.E. First St., Pampano Beach, FL 33061. t0 Wire-Wound Draw Down Bars available from R. D. Specialties, P.O. Box 206, Webster, N Y 14580, or equivalent may be used. 9.n 9-1 reflUy peodi metto D llf 9-2 9.2 colon tion c be ag 9.2 Evah accep refere geom viewi to be opaqi with 9.2 menu the st is agi encet small betwt such evali instr with 9.J 9.. read) appli 9.3 danci 9.4 9.4 coate with 9.4 coil-c D 14 ness) 9.5 9.5 indus propt tests mane 574 DUP050297755 # D 3794 ds ofthe bar. Without rotating the bar, draw it down the [ of the substrate at a uniform speed, so that a uniform i is produced. Draw-down speed is dependent on the iology and quality of the coating being tested. formxtsure ersion :h the there |&J Wet Film Thickness--Determine the wet thickness of ^applied .coating in accordance with Method D 1212. |(j Bake Schedule--Bake the panel at a time and temper- to meet a metal temperature range agreed upon en the producer and user. ersion levant physical Properties of Cured Coating entra- |,1 Dry Film Thickness--There are several methods cur- ose as being used for determining dry film thickness. De- tions. on the substrates being checked, the following ictices Ifehods should be considered: Test Methods D1400, ety of `*f!86, and D 1005. many weight thods p Color: 2.1 The color difference between two homogeneously ibred opaque films may be determined by visual evalua tor by instrumental means. The color standard used shall Ufiagreed upon between the producer and user. t>s on |2.2 Color Differences of Opaque Materials by Visual jnver- m -Visual comparison of color is fast and often nd the pttptable although numerical values are not obtained. The at dip ^ raced method covers the spectral, photometric and --Do ing on paetric characteristics of light source, illuminating and pisg conditions, size of specimens and general procedures ||e used in the visual evaluation of color differences of |^ue materials. Determine color difference in accordance |Practice D 1729. bstrate Jgs by ?2.3 Color Difference of Opaque Material by lnstruEvaluation--Color difference between a product and ^standard can be measured by instrument. The tolerance xmted, e used Avoid ted by fceed upon between the producer and user. The refer- P method covers the instrumental determination of P color differences observable in daylight illumination pen nonfluorescent, nonmetameric, opaque surfaces |as coated specimens. If metamerism is suspected, visual ystrates wn the > degas erature erature en the tainlcss jteveirt ; d**J -quired Btion (9.2.2) should be used to verify the results. Make ^mental measurement of color difference in accordance 11 Test Method D 2244. J-5 Gloss: 1^-1 Gloss in the coil industry is generally determined by at angles of 20, 60, or 85 deg and in some j'jfations by 60/85-deg or 60/20-deg relationships. ' Determine gloss of a coil-coated material in accor^th Test Method D 523. Hi Hardness: BM.1 Pencil Hardness--Determine the hardness of a coil, ^material by the pencil hardness method in accordance "Test Method D 3363. :d on a ipPlie* Indentation Hardness--Determine the hardness of a "?ated material in accordance with Test Methods using either Method A (Knoop indentation hardJ.w Method B (Pfund indentation hardness). ^ flexibility: j in tfe ro There are several flexibility tests used in the coil all giving indications of what the fabrication kes of the coatings are going to be. The most common ^ are impact, wedge bend, T bends, and conical ^flexibility. V FIG. 1 0T, IT Bend 9.5.2 Impact--Determine the impact resistance of a coilcoated material in accordance with Test Method D2794. 9.5.3 Wedge Bend--Determine the wedge bend flexibility in accordance with Test Method D 3281. 9.5.4 Conical Mandrel--Determine the conical mandrel flexibility in accordance with Test Methods D 522. 9.5.5 T Bends: 9.5.5.1 Summary of Method--T bend flexibility is a means of evaluating film flexibility and correlating T bends to fabrication properties, by examining the individual T bends for fracturing and tape adhesion of the coating on each bend. The bends are classified 0T, IT, 2T, 3T, etc., with a 0T bend being defined as a 180 deg bend, (paint on the outside of the bend) pressed flat so there is no space between the metal and the bend (Note 1). The IT bend is made by wrapping or bending the metal around the first bent (OT) so that one thickness of metal is between the new wrap, this bend is pressed flat so there is no space between the metal and the bend. This process is repeated to produce the number of T bends required. (See Fig. 1.) The type of metal substrate to be used, whether or not the bends are to be made with or against the grain of the metal, the designation for identifying T bends and the temperature at which the bends will be made should be agreed upon between the producer and user. NZ[' 1--This is the preferred identification of T bends, however, another method is used based on the inside radius of the bend and is Vi of the preferred designation. 9.5.5.2 Apparatus--Brake form machine.11 9.5.5.3 Procedure--Place the panel to be tested into the bed of the brake face, coated side down. Bend panel 180 deg at a uniform rate and press panels flat so there is no space between the metal and the bend, this is the OT bend. Repeat this process to achieve the desired number of T bends. Examine the T bends under 10-power magnification and report the degree of fracturing on each bend based on a rating system agreed upon between the producer and user. Tape each bend with a tape12 agreed upon between the producer and user. 9.5.5.4 Report--Report the degree of pick off on each bend in a manner agreed upon between the producer and user. 9.6 Adhesion--Determine the tape adhesion of coil mate rials in accordance with Test Method D 3359. 9.7 Pressure Marking and Blocking--Determine pressure marking and blocking resistance of coil-coated materials in accordance with Test Method D 3003. 9.8 Overbake--Determine the effect of overbaking a coil coating material in accordance with Practice D 2454. 11 Di Arco Brake form available from Di Arco Manufacturing. Lake City, MN. 12 Scotch Brand Acetate Fiber Tape No. 710 manufactured by Minnesota Mining and Manufacturing Co., St. Paul, MN., has been found suitable for this purpose. 575 % DUP0502 97756 # D 3794 9.9 Detergent Resistance--Determine the detergent resis tance of an organic coating for the appliance industry in accordance with Practice D 2248. 9.10 Stain Resistance--Determine the stain resistance and effect of household chemicals on a coil-coated finish in accordance with Method D 1308. 10. Exterior Durability and Accelerated Tests 10.1 Outdoor Exposure: 10.1.1 While the accelerated tests given elsewhere in this practice are intended to enable prediction of probable performance, actual outdoor exposures should be made on coatings intended for exterior use. The usage ofpaint systems in the coil area and the liability connected with these systems is so varied that no one set of conditions (length, location, and manner of exposure) can be given in this practice to cover all situations. These conditions, as well as the type of substrate, pretreatment, bake schedule, etc., should be agreed upon between the producer and the user. 10.1.2 Throughout the outdoor weathering tests, several properties should be evaluated periodically or at time inter vals agreed upon between the producer and user in accor dance with the following methods: 10.1.2.1 Blistering--Test Method D 714. 10.1.2.2 Chalking--Test Method D 659. 10.1.2.3 Checking--Test Method D 660. 10.1.2.4 Cracking--Method D 661. 10.1.2.5 Rusting--Method D 610. 10.1.2.6 Corrosion--Method D 1654. 10.2 Accelerated Durability: 10.2.1 Salt Spray Resistance--Salt spray testing of coat ings may be helpful in determining their resistance to failure in service under conditions of high humidity and salt concentrations. Under the accelerated conditions of the laboratory test, the temperature, pH, concentration of the salt solution and other physical parameters can be con trolled. The selection of substrate, pretreatment, the coating system, the manner in which the coating is scribed, the location or position of the panels within the cabinet, the length of the test, the inspection of panels and method of reporting results must be agreed upon between the producer and user. Test for salt spray resistance in accordance with Method B 117. 10.2.2 Acidified Salt Spray--The acidified salt spray is used in the coil industry as a more accelerated test (com pared to regular salt spray) for evaluating corrosion resis tance of coatings over aluminum. Determine the acidified salt spray resistance of a coating in accordance with Method B287. 10.2.3 Humidity--Determine the humidity resistance of coil-coated material in accordance with Practice D 2247. 10.2.4 Water Immersion--Determine the resistance of a coil-coated material to water immersion in accordance with Practice D 870. 10.2.5 Accelerated Weathering--The intention of the ac celerated weathering test is to cause the degradation of coating films to occur much faster than in natural weathering in various field conditions, The apparatus produces more rapid, but not necessarily the same type of failure of films as does natural sunlight because of its higher level and larger peaks of UV irradiation. Materials which absorb at wave lengths where the peaks in UV occur will degrade more rapidly than those that are transparent to those wavelengths. Most, but not all, organic binders are especially sensitive to radiation below 300 nm, and in some cases, no realistic evaluation of weathering properties can be expected. For these reasons, correlation between natural and accelerated weathering is not always obtained. Whenever possible com parisons should be made with materials having similar vehicles and known durability. Conduct accelerated 'weath ering testing on coil-coated finishes in accordance with Practices D 822 or D 3361 (Note 2), or method agreed upon between producer and user. N\]' 2--Practice D 3361 does not use filters and the specimens areSJ exposed to UV below 300 nm. 10.2.6 Filiform Corrosion Resistance--Filiform corrosion, ,, is a type of corrosion that occurs under single-coat systems- , on a metal substrate and is characterized by definite thread-,' like structure and directional growth. When filiform corro sion occurs on residential siding the esthetic value of thejil siding is reduced since the corrosion cannot be washed off. Determine the susceptibility of a coi! coated material to thisi. type of corrosion by Test Method D 2803. The American. Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, either reapproved or withdrawn. Yourcomments are tovited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee which you may attend. If you feet Wia( your comments have not receded a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 576 DUP050297757 ce vtth Designation: 0 3806 - 90a ipray i5 [ (tom- n rev\ cldifiet Wethod Standard Test Method of Small-Scale Evaluation of Fire-Retardant Paints (2-Foot Tunnel Method)1 ime (,, >47 This standard is issued under the fixed designation D 3806; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year ofiast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. ce of a ce Hiii] Sgjjjpe the jv. ion t,l |`- This test method determines the protection a coating gpjsits substrate and the comparative burning charactert!of coatings by evaluating the flame spread over the thenng : more ilms j, large: wa\e- n oto jf|ce when ignited under controlled conditions in a small JnnJ This establishes a basis for comparing surface- I Nftrmv characteristics of different coatings without specific SjjjmKlv`i:.tion of all the end-use parameters that might affect .jijfji-c-burnmg characteristics under actual fire conditions. 1P In addition to the experimental flamespread rate, the ;ngt is. five to selistic 1' Tor prated ! cora- fgj of panel consumed, time of afterflaming and after- & char dimensions and index, and height of intuinesnfsa.y be measured in this test. However, a relationship tf^etild n jt be presumed among these measurements. t*3 This standard should be used to measure and describe jpoperties of materials, products, or assemblies in re- imilar Veath' with' s,to heat and flame under controlled laboratory condijpand should not be used to describe or appraise the fire .upon SEpr fire risk ofmaterials, products, or assemblies under Bpiire conditions. However, results of this test may be 2.2 Federal Standard: Fed. Spec. TT-V-119 Varnish, Spar, Phenolic Resin5 3. Significance and Use 3.1 A number of laboratory procedures are used to evaluate the effectiveness of fire-retardant and fire-resistant treatments and coatings. In general, these methods measure the three stages of fire development: (7) ignition; (2) flame spread (rate of growth of the fire); and (3) conflagration extent While all three are of extreme importance, flame spread has been recognized as the main factor associated with testing fire-retardant coatings. 3.2 Flame spread ratings based upon Test Method E 84 have acquired common acceptance by regulatory agencies, but such large-scale tests are seldom practical during the development or modification of a fire-retardant coating. 3.3 This test method provides the relative flame spread of experimental coatings using small test specimens. By cali brating the 2-foot tunnel with: Test Method E 84-rated d ns elements of a fire risk assessment which takes into Stint all of the factors which are pertinent to an assessSg!>f the fire hazard of a particular end use. fire-retardant paint, results obtained by this test method should be indicative of those obtained with a large specimen in the Test Method E 84 tunnel. standard does not purport to address the safety Mems associated with its use. It is the responsibility ofthe W&f this standard to establish appropriate safety and 4. Apparatus Wk practices and determine the applicability ofregulatory tjmtions prior to use. 4.1 Flame Tunnel6 (see Fig. 1A)--two-foot (610-mm) flame tunnel consisting of asbestos-cement board mounted i-ferenced Documents on an iron framework and supplied with natural gas fuel of uniform quality. 1 . {STM Standards: 220 Specification for Rat Asbestos-Cement Sheets2 4.1.1 The framework is constructed of Vs by 1 by 1-in. (3 by 25 by 25-mm) angle iron, the top of which provides a 24 344 Test Method for Relative Hiding Power of Paints by t',e Visual Evaluation of Brushouts3 by 4-in. (610 by 100-mm) specimen holder inclined at 28to the horizontal. The framework is mounted on a 10 by 24 by 47^ Test Method for Density of Paint, Varnish, Lac- Win. (250 by 610 by 13-mm) steel base. The specimen qiu. i, and Related Products3 holder is elevated 7% in. (185 mm) above the base at the 196 Test Methods for Rheological Properties of Non- lower (fire) end and 187/s in. (480 mm) at the upper (flue) Newtonian . Materials by Rotational (Brookfield) end. \ iscometer3 4.1.2 The fire end and sides of the tunnel are covered to est Method for Surface Burning Characteristics of the extent shown in Fig. 1, with `4-in. (6-mm) asbestos- Building Materials4 cement board7 or Win. (6-mm) inorganic reinforced-cement This test method is under the jurisdiction of ASTM Committee D-1 on Paint ^delated Coatings and Materials and is the direct responsibility of Subcom" < .:22 on Health and Safety. it edition approved Oct. 26, 1990. Published December 1990. Originally is D 3806 -79. Last previous edition D 3806 - 90. r/ Book ofASTM Standards, Vol 04.05. 7 Book ofASTM Standards, Vol 06.01. tmuat Book ofASTM Standards, Vol 04.07. 3 Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. 6 Flame tunnels manufactured to similar specifications arc available from Custom Scientific Instruments, 13 Wing Drive, Cedar Knolls. NJ 07927 and Monsanto Co., Functional Products, Special Chemicals Div., 800 N. Lindbergh Blvd., Si. Louis, MO 63167. 7 Transite, manufactured by Manvillc Corp., Denver CO 80217 has been found satisfactory for this purpose. 577 DUP0502 97758 # D3806 Item Base Plate Framework Side and Front Panels Side Glass Burner Gas Conlrol Valve (not shown) Gage, Gas (not shown) Materials of Constrjctlon and Equipment Ust Description item No Item Description % x 10 x 24 Steel plate % x lx Angle Iron throughout Va. Transite or Chem-FII 1Q0S or 100 He cut to specifications Vo X 2 x 24 Polished Vycor cut as shown Artificial Gas Model Ve Orifice, 1" Ptpe size, outlet 3 oz/in2 F G H l J K Glare Shield Ignition Transformer Spark Switch Ceramic insulator Spark Wire Thermocouple Vie x 2'A x 22 Metal sheeting 115 V, 60 $z, 5000 V, 20 A secondary Push button type Via OD Nichrome Megopak Type J, totally shielded 0-30 oz/in2 Dial Recording Potentiometer 115 V, 60 Hz, 0-300C, Type J concl Note: All Dimensions Expressed In Inches Unless Otherwise Noted. 1 SECTION A-A In. Vie %2 Vs Vi Vi 1 V/z 2% 2% EgQNXJttBtt METRIC EQUIVALENTS mm in. 1.6 3 2.4 4 3.2 7 6.4 7% 12.7 25.4 38 10 loyz 184b 57 22 70 24 TIG. 1 Flame Tunnel SIDEujaOt mm 76 102 178 137 254 267 430 560 610 BEAR VIEW board8 attached to the inside of the angle iron framework. The open flue end and the cut-out sides allow a natural draft through the tunnel. Additional air access is provided by a 1-in. (25-mm) hole drilled in the cover at the fire end, centered and 4Vi in. (115 mm) above the base. 4.1.3 An observation window made of a 2-in. (50-mm) wide strip of '/s-in. (3-mm) polished heat-resistant sheet glass9 is located just below the specimen holder, extending the full length of the tunnel, 24 in. (610 mm). This glass is 8 Chem-Fi! JOOS and J00H, nominal 100 to 110 Ib/ft3 (1600 to 1760 kg/m3), Chem-Ftl Corp., 100 Spence Lane, Nashville, TN 37210 have been found suitable for this purpose. 9 Quartz or high-silica glass has been found satisfactory for this purpose. marked by any appropriate method at 1-in. intervals from 4 to 22 in. A 22 by 2`A by '/[6-in. (560 by 55 by 2-mm) sheet metal shield is attached above the window, slanting down wards at an angle of 60" to shield the observation window. The angle iron panel holder is notched along the bottom or supporting lip ofthe angle at 1-in. (25-mm) intervals to assist in the measurements of the flame advance. N_`' l--A rule may also be mounted outside the observation window to help measure the flame advancement. 4.1.4 A %2-in. (2.5-mra) hole is drilled in the side of the specimen holder immediately above the center of the burner to allow insertion of a thermocouple. 4.1.5 The tunnel should be ptaced in an area as free from 578 DU PO50297759 # D 3806 TABLE 1 Densities and Panel Weights of Various Woods (Conditioned at Relative Humidity SO 6 % and 73.5 3.5F (23 2C) for 14 days) Si1-1 Type of Wood Density (9 to 10 % Moisture), Ib/ft3 (kg/m3) Weight of 3% by 23Vo by v* in. Panel, g ' < ; \r * fjjjfe Red cedar Douglas fir White pine-Ponderosa pine ' Southern yellow pine Redwood 21.4 to 22.4 (345 to 360) 29 to 35 (465 to 560) 22.4 to 26.4 (360 to 420) 31 to 37 (495 to 590) 27.2 to 28.2 (435 to 450) 130 to 140 160 to 215 140 to 160 190 to 225 165 to 175 as possible with facilities for removal or escape of iistion products. (Standard laboratory hood with forced off during test.) %Bumer' 8.5 in. (215 mm) high with 40-mm ieter.lO-mm thick grid for use with natural gas. The :r is placed 2'A in. (57 mm) in from the fire end of the nel and 1 in. (25 mm) below the bottom side of the le holder, that is, 1 Vs in. (30 mm) from the bottom of ipecimen. See Fig. 1. ,2--Artificial gas or liquid petroleum (LP) gas may be used, but IPis designed for these types of gases must be used. Ignition Transformer, or other suitable ignition :e, to generate a spark through a 'Ae-in. (2-mm) |pme wire to the burner barrel. The transformer is lied by a push-button type spark switch. U Gas Supply, of uniform quality controlled by a lire-flow pressure regulatory valve (0 to 6 in. (0 to 152 water) and a gas flowmeter (0.6 to 5.0 SCFH). lb Insulating and Fire Resistant Backingfor Test Panels fisting of 3% by 23%-in. (100 by 605-mm) pieces of jm. ;(13-mm) asbestos-cement board or inorganic reingP cement board and 'A-in. steel plate applied one above pfiiher with asbestos cement or the inorganic reinforced |nt board placed directly on top of the test panel. $. Thermocouple11 totally shielded (see Note 3) installed Ugh the hole in the side of the specimen holder so that its rests on the back, cool side, of the test panel. Mab' 3--Some commercial tunnels6 are supplied with more than Uihermocouple. 4:.7 Recording Potentiometer, 0 to 300C range. 4r8 Audible Timer, set to sound at 15-s intervals to itdicate the time for flame-front measurements. jjjR9 Constant Temperature and Humidity Room or Cabmi' maintained at 50 5 % relative humidity and 73.5 JsF (23 2C)i Test Panels IS. I Test Panels--See Table 1 for a list of various woods ptd their densities, Wood, 'A by 3% by 237/s-in. (6 by 100 by jp-mm) close grained, as nearly edge grain as possible and |ee from knots and imperfections. The panels should be , jlid wood with surfaces planed and sanded (see Note 4). , Kiln-dry test panels to contain not more than 10 weight % of ii. moisture on an oven dry basis. Ncd' 4--Douglas fir, Vi-in. (6.3-mm) 3-ply, marine-grade plywood may be used upon agreement between manufacturer and user. Asbestoscement board, steel, or concrete may be used upon agreement between manufacturer and user. 5.1.1 Prior to coating, condition test panels for 14 days in the controlled atmosphere of 50 5 % relative humidity and 73.5 3.5"F (23 2C) to a 9 to 10 % moisture content. Refer to Table 1 for the density and weight per panel ofeach listed wood. 5.1.2 Seal the ends of the panels with two coats of varnish conforming to Fed. Spec. TT-V-119 after conditioning. Allow each coat of varnish to air-dry 18 to 24 h. 6. Calibration Standards 6.1 Zero-Flame Spread-- Asbestos-cement board, Type F conforming to Specification C 220, Vr by 3% by 23% in. (13 by 100 by 605 mm), conditioned as in 5.1.1. Nef' 5--Inorganic reinforced cement board, 'A-in. (6.3-mm) thick may be substituted for asbestos cement. 6.2 Fire-Rated Standard--A test panel, similar to that ' used with test coatings, coated with Test Method E 84 rated paint at the manufacturer's recommended spreading rate and conditioned as in Section 7. Ngh' 6--Do not use paint beyond manufacturer's stated shelf life. 7. Preparation of Test Panels 7.1 Thoroughly mix the coating under test by a suitable means until it is uniform in composition and consistency. Test Method D 2196 describes a suitable preparation proce dure. 7.2 Determine the density of the coating in accordance with Test Method D 1475 in pounds per gallon (or grams per millilitre) for calculating the weight of the coating to be applied to the panel to comply with the specified spreading rate. 7.3 Brush apply the coating to conditioned test panels in as uniform a manner as possible to obtain the specified spreading rate. A suitable procedure appears in Test Method D 344. Application may be by other conventional means and in as many coats as required to obtain the necessary weight of coating or desired wet- or dry-film thickness. 7.4 Calculate the weight of coating to be applied using the following equation: (3% X 23%)> W - 144 SR - X 454 jSfc,. 10 Fisher Burner Catalog No. 3-902 from Fisher Scientific Co. has been found Ipjsatjsfactory for artificial gas. Fisher Burners No. 3-900 and 3-902 may be used for |P?Ural gas and LP gas, respectively. 11 Megopak Type J thermocouple has been found satisfactory for this purpose. where: W weight of applied wet coating, g, D coating density, lb/gal, and SR = spreading rate, ft2/gal. 579 DU P0502 97760 # D 3806 7.4.1 Use the following equation when metric units are employed: Or where: W = weight of applied wet coating, g, D = coating density, g/mL, and Sr = spreading rate in m2/L. 7.5 Dry the coated panels under standard conditions (4.9) until equilibrium weight is obtained, allowing sufficient time for the complete evaporation of solvents, any curing that might be required by the material, and for the attainment of equilibrium moisture content. Forty-eight hours are nor mally sufficient except for certain coatings that may require longer periods because they trap solvent or contain solvents that evaporate very slowly. 7.6 Apply and cure non-air-drying coatings as recom mended by the supplier and condition as specified in 7.5. 8. Calibration of the Tunnel 8.1 Calibrate the tunnel prior to each day's operation with the calibration standards described in Section 6. 8.1.1 Place the zero flame-spread standard in the holder, smooth side down, and back it with the backing plate (4.5). 8.1.2 Open the gas valve and adjust to a pressure of 3 oz/in.2 (1.3 kPa) and a constant flow of 4.8 ft3/h (38 mL/s), and actuate the interval timer. Nij' 7--These conditions are specified for a natural gas supply providing 1055 BTU/fP (40 MJ/m1). For any other gas supply, adjust flow to provide 5085 BTU/h (1490 J/s). 8.1.2.1 When the timer sounds, ignite the burner using the ignition transformer. Observe the flame front, measure in inches and record at 15-s intervals the flame position by aligning the notches in the bottom of the specimen holder with the markings on the observation window. 8.1.3 Record the extreme tip ofthe flame advance (flame front) on the panel surface, disregarding flame extending up the tunnel but completely on the angle iron support. After a total test period of 4 min, extinguish the burner. 8.1.4 Calculate the mean of the three highest consecutive readings of the flame advance of the zero-flame spread standard La. 8.2 Repeat the calibration procedure using a fire-rated standard (6.2). Designate the mean of the three highest consecutive readings of the flame advanced as Ln. The difference between the mean readings for the zero flamespread standard and the fire-rated standard (LK - La) is directly related to the Test Method E 84 flame-spread rating of the rated standard {FsR).9 9. Procedure for Determination of Flame-Spread Rating 9.1 Remove a test panel (Section 7) from the controlled atmosphere, weigh immediately, and then mount in the specimen holder, coated-side down. Insert the thermocouple through the hole in the holder (4.6) so that its tip is directly above the center of the burner and resting on the back, or uncoated side, of the test panel. Back the panel with the asbestos-cement board and steel backing. 9.2 Apply the flame and determine the advance of the flame front in the same manner as the calibration procedure (Section 8), Except allow the burner to operate for an additional 60 s after making the last of the 15-s readings before extinguishing the burner. Designate the mean of the three highest Consecutive readings of the flame advance of the specimen during the 4-min test period as Ls. 9.3 Repeat the determination with at least five panels. 10. Calculation 10.1 Calculate the experimental flame-spread rating using the following equation: where: (t. Er ~ -- 4.) La x Fsi Fk' = flame spread of specimen, Ls = meajn of three flame advance readings of specimen, in. (jmm), La = mean of three flame advance readings of zero flanfe-spread standard, in. (mm), Lr = mean of three flame advance readings of rated standard, in. (mm), and Fs r = flame-spread rating of rated standard. 10.2 Calculate the mean ofthe replicate panels, roundinu off to the nearest five units. 11. Optional Measurements 11.1 Afterfiaming Time--Observe and record the time in seconds that flaming continues on the face of the test specimen after the burner has been extinguished. Report as afterfiaming time. 11.2 Afterglow Time--Observe in subdued light and record the additional time in seconds that the surface of the1 test specimen continues to emit light (glows) after the flame has gone opt. Report as afterglow time. 11.3 Patiel Consumption--After the completion of the flame-spread test (Section 9), replace the specimen in the' constant aftmosphere. (see 5.1.1) for not less than 72 h Reweigh the panel and determine the weight loss in grama Report loss as panel consumption. 11.4 Degree of Intumescence--Measure the height of intumescence (foam formation) in millimetres at the point on the specimen that was directly above the burner. Report the heightias intumescence. 11.5 Insulation Value--Measure the initial panel temper ature in djegrees Celsius or Fahrenheit and subtract it frem the maxiniium temperature observed during the flame-spread test (Sectipn 9). Report the difference as AT. 11.6 Char Dimensions and Index--Cut the panel inf four rectangular pieces using a fine-toothed saw so that 1i.' cuts intersect at the point of flame impingement (directly over the burner). Measure in centimetres the maximum width of (fharring of the wood found below the paint film uu the lateral cut. Likewise, measure the maximum length of charring found on the longitudinal cut. Measure the max imum depth to which charring has penetrated as evidenced ' on either cut. Determine the char index by multiplying the1 maximum char width, length, and depth. 12. Report 12.1 Experimental Flame Spread--Report the following information: 580 i' 1 V r DU PO 502 97761 D 3806 g usm nding J1.1 The calibration values of LR and La (Section 8), Type of substrate used, (2,1.3 Number of test panels, rt^|2.1.4 Mean spreading rate, *'`.5 Pressure, flow rate, and type of gas fuel, Mean Ls value for each panel (Section 9), and Mean flame-spread value (fSE) for each material test (Section 9). '. Optional Measurements--Report may contain the Bowing information: 12.2.1 Panel Consumption--Mean initial and final weight 15>}'Boated specimens and mean weight loss in grams (11.3), > 12.2.2 Afterflaming time in seconds (11.1), Hpl2.2.3 Afterglow time in seconds (11.2), 8|2.2.4 Height of intumescence in millimetres (11.4), I Hp2.2.5 Insulation Value--Initial and maximum tempera- es, and temperature difference (AT) (11.5), and &12.2.6 Char Depth and Volume--Maximum width, h, and depth of charring of wood in centimetres and the index in cubic centimetres (11.6). 1 Precision and Bias 13.1 Precision: 113,1.1 Nonuniformity of test panels (both in the wood rd in the coating), variations in fuel supply and rate, and TABLE 2 Repeatability Flame-Spread Ratings Standard Deviation Coefficient of Variation 0 to 25 25 to 75 75 to 135 0 to 135 1.2 9.6 3.1 6.2 3.65 3.5 2.85 4.6 * This information was derived tram Journal of Paint Technology, Vol. 39, No. 511,1967, p. 495. operator error are the chief sources of error in operation of the 2-foot (610-mm) tunnel. 13.1.2 The degree of repeatability is dependent on the level of flame-spread ratings. Table 2 shows that while the standard deviation of duplicate results increases with an increase in ratings, the coefficient of variation decreases by a factor of more than 2.0. 13.1.3 The standard deviation in Table 2 relates to the maximum difference that would be expected between dupli cate panels; that is, a second result in the flame-spread range from 0 to 25 should fell within 4.8 units (2.8 x 1.2) at the 95 % confidence level 13.2 Bias--The procedure in this test method for mea suring flame spread has no bias because the value of flame spread can be defined only in terms of a test method. 14. Keywords 14.1 fire-retardant; flame spread; paints; tunnel method and if the Same The American Society tor Tooting and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ere entirely their own responsibility. This standard. Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if riot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should, be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. iperirom read: s ring 581 Han DUP0502 97762 Designation: D 3842 - 86 (Reapproved 1991) Standard Guide for Selection of Test Methods for Coatings for Use in Light-Writer Nuclear Power Plants1 This standard is issued under the fixed designation D 3842; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of lost revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revirion or reapproval. 1. Scope 1.1 This guide is intended to provide a common basis in the selection of test methods that may be required to evaluate and qualify protective coatings (paints) for use m a light-water nuclear power plant, and all the listed items are for Coating Service Level I application. It lists and describes tests to be conducted on all coatings specified for this service,. 1.2 This guide also lists the specifications and their scopes that describe evaluation tests for these coating systems. 1.3 Coating Service Level I pertains to those coating systems whose failure could impair the operation of the engineered safety features that are essential for preventing the possible consequences of postulated accidents that could cause undue risk to the health and safety of the general public. Coating Service Level I applies principally to the interior surface of the primary containment for both Pressur ized Water Reactors (PWR) and Boiling Water Reactors (BWR) and to the structures and equipment contained therein. Coated surfaces include, but are not limited to, carbon steel, stainless steel, galvanized steel, aluminum, and masonry. 1.4 Requirements for coatings applied to other areas shall be assigned at the option of the owner or his designated representative. It is intended that this standard be incorpo rated in specifications, by reference, on the basis of owner requirements. 1.5 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility ofthe user ofthis standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D3911 Test Method for Evaluating Coatings Used in Light-Water Nuclear Power Plants at Simulated Design Basis Accident (DBA) Conditions2 D3912 Test Method for Chemical Resistance of Coatings Used in Light-Water Nuclear Power Plants^ D4082 Test Method for Effects of Radiation on Coatings Used in Light-Water Nuclear Power Plants2 D4256 Test Method for Determination of the Decontaminability of Coatings Used in Light-Water Nuclear Power Plants2 3. Significance and Use 3.1 This guide covers methods of testing coatings for use in light-water nuclear power plants. 4. Test Methods 4.1 Test Method D3911--This test method establishes procedures for evaluating protective coating systems test specimens under simulated Design Basis Accident (DBA) Conditions. Included is a description of conditions and apparatus for temperature-pressure testing, condition for radiation testing, and procedures for preparing, examining, and evaluating the samples after testing. 4.2 Test Method D3912--This test method establishes; procedures for the evaluation of the chemical resistance of coatings used in light-water nuclear power plants. 4.3 Test Method D 4082--This test method establishes a standard procedure for evaluating the lifetime radiation tolerance of coatings to be used in nuclear power plants. 4.4 Test Method D 4256--This test method establishes procedures for determining and ranking the ease of the decontaminability of coatings used in nuclear power plants. ir-i jgablqj S-T '1 ! 1 |Sj6sis) Iv, ork i IIM ,, `he tl 1 Hg&pgj 1 This guide is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.02 on Service and Material Parameters. Cunrent edition approved Sept. 29, 1986. Published November 1986. Originally published as D 3842 - 80. Last previous edition D 3842 - 80. 2 Annua! Book ofASTM Standards, Vol 06.01. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either tor revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you fee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Rece St., Philadelphia, PA 19103. ? IjU jSxcrftfc ggSubW /I 582 DU P050297763 I Designation: D 3843 - 89 Standard Practice for Quality Assurance for Protective Coatings Applied to Nuclear Facilities1 This standiird is issued under the fixed designation D 3843; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearoflast revision, A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. ed in atings it mgs econicleai ishes , test )BAl and | for ?iqg, W:S .Pd shes I'tf C:'f . 6s a-4'lmiirmK lion - j shes itipl ats. . Scope iji This practice provides a common, basis for, and pecifically comprises quality assurance requirements appliahle to, safety-related protective coating work in Coating |mceLevel I areas of nuclear facilities. ' p-1.2 Applicable portions ofthis practice may be used as the j.s for limited quality assurance for protective coating Ipk in Coating Service Level II areas of nuclear facilities. This standard may involve hazardous materials, Rations, and equipment. This standard does not purport to ^$Iess all ofthe safety problems associated with its use. It is 'ftresponsibility of the user of this standard to establish fy'Mpprleue safety and health practices and determine the fyicability of regulatory limitations prior to use. Referenced Documents ill ASTMStandards: | 3842 Guide for Selection of Test Methods for Coatings jjjLfor Use in Light Water Nuclear Power Plants2 |t4227 Practice for Qualification of Journeyman Painters I for Application of Coatings, to Concrete Surfaces of || Safety Related Areas in Nuclear Facilities2 >4228 Practice for Qualification of Journeyman Painters p'for Application of Coatings to Steel Surfaces of Safety . Related Areas in Nuclear Facilities2 >4537 Guide for Establishing Procedures to Qualify and Certify Inspection Personnel for Coating Work in Nu clear Facilities3 !? ANSI Standards: if5.2 Quality Assurance Program Requirements for Nui'clear Power Plants4 I'f3 Code ofFederal Regulationsf IjjO CFR 50, Appendix B: Title 10, Chapter 1, Energy, Part 50, Licensing of Production and Utilization Facilities, Appendix B, Quality Assuraiice Criteria for Nuclear Power Plants and Fuel Reprocessing Plante BIO CFR 21 Reporting of Defects and Ncmcompliances |'| l This practice is under the jurisdiction of ASTM Committee D-33 on rective Coating and Lining Work for Power Generation Facilities and is the ^.responsibility of D33.03 on Quality Systems. Current edition approved Feb. 24, 1989. Published April 1989. Originally itiblished as D 3843 - 80. Last previous edition D 3843 - 80. Annual Book ofASTM Standards, Volz 06.01 and 12.01. 3 Annual Book ofASTM Standards, Vo) 06.01. 4 Available from American National Standards Institute, 13th Floor, II W. |2nd St., New York, NY 10036. * Available from the Superintendent of Documents, tXS. Government Printing , Washington, DC 20402. 3. Terminology 3.1 Description of Terms Specific to This Standard: 3.1.1 certification--the written documentation of the qualification of personnel or material. 3.1.2 coating applicator--an organization or individual responsible for applying a protective or decorative coating, system. ; 3.1.3 coating (paint)--a liquid, liquifiable, or mastic com position that is converted to a solid protective or functional adherent film after application as a thin layer. 3.1.4 coating manufacturer--an organization responsible for manufacturing coating materials. 3.1.5 coating system--a polymeric protective film con sisting of one or more coats, applied in a predetermined order by prescribed methods. 3.1.6 coating wor/c--an all-inclusive term to, define all operations required to accomplish a complete coating job. The term shall be construed to include materials, equipment, labor, preparation of surfaces, control of ambient conditions, application and repair of coating systems, and inspection. 3.1:7 Code ofFederal Regulations (CFR)--the rules and regulations of the United States Federal Government. The code is subdivided into titles, with Title 10 (10 CFR) applying to energy, 3.1.8 deviation--a departure of a characteristic from es tablished procedures or specified requirements. 3.1.9 documentation--any written or pictorial informa tion describing, defining, specifying, reporting, or certifying activities, requirements, procedures, or results. 3.1.10 inspection--a phase of quality control which by means of examination, observation, or measurement deter mines the conformance of materials, supplies, components, parts, appurtenances, systems, processes, or structures to predetermined quality requirements. 3.1.11 inspection agency--a person or persons authorized by the owner or owner's designee to verify conformance of the coating work. 3.1.12 nonconformance--a deficiency in characteristic, documentation, or procedure that renders the quality of an item unacceptable or indeterminate. Examples of noncon formances include: physical defects, test failures, incorrect or inadequate documentation, or deviation from prescribed processing, inspection, or test procedures. 3.1.13 owner--the person, group, company, or corpora tion who has or will have the license for the facility or installation. 3.1.14 owner's designee--a person or persons authorized by the owner to act in his behalf. 583 DU P0502 97764 < D 3843 3.1.15 vendor--any individual or organization who fur nishes items or service to a procurement document. 4. Significance and Use 4.1 Quality assurance, as covered by this practice, com prises all those planned and systematic actions necessary to provide adequate confidence that safety-related coating work in nuclear facilities will perform satisfactorily in service. 4.2 Coating Service Level I applies to areas where coatings failure could adversely affect the operation of post-accident fluid systems. With some exceptions, Coating Service Level I applies to coatings inside primary containment. 4.3 Coating Service Level II applies to areas where coat ings failure could impair, but not prevent, normal operating performance. The primary function of Service Level II coatings is to provide corrosion protection and decontaminability in those areas outside primary containment subject to radiation exposure and radionuclide contamina tion. 4.4 It is not practical to impose all the requirements of this practice on certain specific items that require only a small quantity of coating material. The owner, consistent with his formal Quality Assurance Program, may accept affidavits of compliance or certification attesting to the quality of a shop or field coating for such items. If required by licensing commitments, uncontrolled (unqualified, nonconforming, or unidentified) coatings shall be identified, quantified, and documented, 4.5 This practice may be incorporated in a project speci fication by direct reference or may be used to provide guidelines for the quality assurance program for coatings, on the basis of the owner's requirements. Effective use of this practice may also require the incorporation of applicable sections in project specifications for coatings on concrete, steel, equipment, and other related items. 5. General Quality Assurance Requirements 5.1 This section defines the general quality assurance requirements necessary for compliance with this practice. These requirements shall apply to all other sections of this practice. 5.2 The owner or the owner's designee shall be responsible for determining whether source inspection or a certificate of compliance attesting to the quality of coating work activity is required. 5.3 The general quality assurance requirements necessary to meet the purpose of this practice provide an acceptable basis for establishing a protective coating quality assurance program. All deviations from or exceptions to these require ments shall be reviewed by and shall be subject to approval by the owner or his designee before implementation. If unapproved deviations are discovered during any phase of the coating work activity, a nonconformance report shall be completed either by the owner, vendor, or owner's designee. The owner or the owner's designee shall approve the disposition of the nonconformance report. Nlm' --Notification ofthe Nuclear Regulatory Commission (NRC) is required by 10 CFR 21 for certain types of defects and noncompliances. 5.4 There are five major activities that shall be controlled and documented as a minimum for Service Level I protec tive coatings applied to nuclear facilities as follows: 5.4.1 Qualification and selection of coating materials, 5.4.2 Coating manufacturing, 5.4.3 Surface preparation of substrates, 5.4.4 Control of coating application, and 5.4.5 Coating inspection. 5.5 The five major activities specified in 5.4 are designed to meet the applicable quality assurance requirements of Appendix B to 10 CFR 50, and of ANSI N45.2. All five of these controlled activities shall have appropriate documenta tion including approved procedures and records to meet the Appendix B and N45.2 requirements. 5.6 The qualification and selection of coating materials shall be evaluated by the owner on the basis of criteria defined in Section 6 of this practice. 5.7 The coating manufacturer shall furnish a quality assurance program describing his methods for quality control' of the specified coatings on the basis of criteria defined id Section 7, which is approved by the owner. 5.8 Should the owner designate an outside coating appli cator to apply the specified coatings, the coating applicator shall provide a quality assurance program based on the criteria defined in Sections 8 and 9, which is approved by the owner. 5.9 Should the owner designate an inspection agency to inspect the application of the specified coatings, the inspec tion agency shall provide a quality assurance program based on the criteria defined in Section 10, which is approved by the owner. 5.10 If application or inspection, or both, are performed under the owner's quality assurance program, procedures shall be established to control these activities. prof 3 11.' 6. Control of Selection and Qualification of Coating Mati rials 6.1 All qualifications of coating materials shall m applicable standards referenced in Guide D3842 to the -fl extent defined by the owner or the owner's designee in design criteria, safety analysis reports, quality assurance program, or other controlling documents. 6.2 The coating manufacturer shall furnish recommended surface preparation and application procedures for each coating system on each substrate as covered by the project" specification including previously coated surfaces as appli cable. The coating manufacturer shall also furnish recom-!r mended storage conditions for each coating material speci-^f fied. 7. Control of Coating Manufacturing 7.1 The coating manufacturer shall maintain a Quality Assurance Program and shall provide adequate documenta tion to show that the quality of a given coating system a' supplied is the same composition (within owner approved manufacturing tolerances) the coating system previously tested for qualification. The coating system shall be requalified if there are significant changes in formulation or end-product properties. The manufacturer shall provide the owner or the owner's designee documentation based on the ; criteria stated in 7.1.1 through 7.1.5. 7.1.1 The coating manufacturer shall provide the puichaser with a product identity certification record for each batch of coating material shipped. As a minimum, the 584 DUP050297765 4eiwli ritena Mu, " nltol j led i$8 'W'l icator tiu >J the mod** 1IIIC1- latt- D 3843 ct identity certification record shall contain the folg infortnation: jtl.l Established acceptance criteria ranges and batch acteristics for weight per gallon and viscosity, |r 1.2 Batch number, it 1.3 Date manufactured, || 1.4 Shelf life expiration date, U.5 Certification (signed by a responsible technical jtger) that the product shipped is the same composition Ifn owner-approved manufacturing tolerances) as the [[act tested for qualification. Separate acceptance criteria may be established for atjon at time of manufacture and for evaluation during hblf life period, but these shall be. separately identified. |,3 Data which is generic to the product and not batch fie (for example, nonvolatile, cure time, pot life, etc.) |be furnished to the owner as requested, but need not be fcated on each product identity certification record. 1,4 Material which has exceeded shelf life may be tluated by testing and the shelf life extended in writing he manufacturer's technical department. Testing for nsion of shelf life shall be performed on an unopened liner removed from the job site storage area, and not a retained laboratory sample. (`l .5 The owner may elect to perform verification testing aducts received to ensure compliance with this practice. Each container shall be labeled with the product ^ nation. The label or container shall bear a batch tlber or other factory marking, permanently affixed, ng the individual lot or batch designation. The date of jlufacture, and the shelf fife expiration date shall appear ately on the label or container. .Retained batch samples from products furnished for '""project shall be kept by the manufacturer for the stated "life. ' Control of Surface Preparation of Substrates 8.1 This section defines the quality assurance requirecius for the surface preparation of bare substrates or of eviously coated surfaces. 3 The surface preparation of substrates or of previously ned surfaces shall conform to the requirements of the iject specification. Treatment of nonqualified or iicompatible concrete primers/sealers and concrete formrtcase agents shall be addressed. 8.3 The project specification shall include inspection fn.thod s to ensure the requirements of the specification are let. is 4 fhe coating applicator shall submit written surface epji ition procedures addressing each substrate to be atod including previously coated surfaces. . 5 The responsible organization shall report daily on surface preparation during each shift for each area of work. 9. Control of Application of Coating Systems 9.1 This section defines the quality-assurance require ments necessary to comply with this practice to ensure that the applied coating system is basically the same as that which was tested for qualification. 9.2 The coating applicator shall follow written owner ac cepted application procedures for applying each coating sys tem on each substrate and on each previously coated surface. The coating manufacturer's latest written application in structions shall be incorporated as part of the procedures. 9.3 All application personnel shall be qualified and their qualification documented in accordance with the applicable quality assurance program and Practices D 4227 or D 4228. 9.4 Receiving, storing, and dispensing ofcoating materials shall be appropriately documented as per established require ments. 9.5 The responsible organization shall report daily on the application work for each shift for each area of work. 10. Control of Coating Inspection 10.1 It is the responsibility of the owner as identified in 5.3 to specify and verify control measures to assure that the inspection of the coating work is adequate to achieve the required quality. Inspection hold points shall be established to ensure in-process inspection results are adequate. The owner or the owner's designee shall be responsible for the inspection activity. In all cases the inspection function shall be properly documented as required by Appendix B of 10 CFR 50 and ANSI N45.2 for record purposes. 10.2 All inspection personnel shall be qualified and certi fied in accordance with Guide D 4537. 10.3 Inspection shall conform to all the applicable re quirements of the project specification and all other appli cable requirements of this document. 10.4 A written daily coating inspection record shall be maintained by the owner. 10.5 In the case of any significant deviation or defective work, the corrective action shall be documented. 10.6 Final acceptance of completed work shall be docu mented. 11. Documentation 11.1 Sufficient quality-assurance records and documents shall be maintained to furnish objective evidence of compli ance with the specifications and the specified quality assur ance procedures. 11.2 Documentation shall be maintained by the owner or the owner's designee as defined in the owner's quality assurance program. 11.3 Distribution of documentation shall be as defined in the quality assurance procedures. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in tWs standard. Users of this standard are expressfy advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 585 DUP050297766 Designation: D 3891 - 90 Standard Practice for Preparation of Glass Panels for Testing Paint, Vamish, Lacquer, and Related Products1 This standard is issued under the fixed designation D 3891; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval A superscript epsilon (c) indicates an editorial change since the last revision or reapprovaL 1. Scope 1.1 This practice covers the preparation ofglass panels for subsequent testing of paint, varnish, lacquer, and related products.12 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 364 Specification for Industrial Grade Xylene3 D1152 Specification for Methanol (Methyl Alcohol)4 D1193 Specification for Reagent Water5 3. Significance and Use 3.1 The procedures described in this practice are designed to provide uniform glass panels for testing of paint, vamish, lacquer, conversion coatings and related products. 4. Reagents and Materials 4.1 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193. 4.2 Solvents--V M & P naphtha, xylene, 2-methoxypropanol, and methanol complying with the appropriate speci fications (see Specifications D 364 and D 1152). 4.3 Glass of the following types may be specified in the applicable test methods: 4.3.1 Window Glass, (float glass) the surface of which is plain and free of irregularities. 1 This practice is under the jurisdiction of ASTM Committee D-i on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.27 on Accelerated Tests for Protective Coatings. Current edition approved Aug. 30, 1990. Published November 1990. Originally published as D 3891 - 80. Last previous edition D 389J - 80. 2 This practice is intended to be equivalent to Method 2021 ofU.S. Federal Test Method Standard 141. 3 Discontinued, see 1982 Annual Book ofASTM Standards, Vol 06.03. 4 Annual Book ofASTM Standards, Vol 06.03. 5 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4.3.2 Clear Plate Glass, not less than 5 mm thick. 4.3.3 Plate Glass that has been ground uniformly on one side with IF carborundum. 4.3.4 Black Structural Glass,6 one side of which has been polished to a smooth, high-gloss surface. 4.3.5 White Structural Glass, one side of which has been polished to a smooth, high gloss. 5. Method of Preparation 5.1 New Panels--Using a dean lintless cloth, wipe the panel with a solvent mixture consisting of equal volumes of V M & P naphtha and xylene or of 3 volumes of V M & P naphtha and 1 volume of 2-methoxypropanol or with watei When all soluble and loosely adhering soil has been washed off, flush with clean solvent Allow panels to dry at room temperature or force dry at a temperature no higher than 300F (15Q"C). After cooling to room temperature, rub with a clean lintless cloth if necessary. 5.1.1 The surface after cleaning shall be water-break free This is determined by momentarily immersing in reagent water one panel of each twenty prepared. If a continuous water film is not retained (that is, the water film breaks), immerse the panel in methyl alcohol to obtain a watefbreak-free surface. After removal, dry at a temperature o: 125 to 200F (52 to 93C) and allow to cool before coating oi storing. 5.1.2 Other combinations or organic reagents that will produce a surface equal in cleanliness to the solvent mixtures , mentioned in 5.1 may be used if agreed upon between the purchaser and the supplier. 5.2 Used Panels--Remove the old paint, using a paint, and varnish remover ofthe organic solvent type or a suitable solvent mixture. Do not use a spatula, sandpaper, or other instrument of treatment that might scratch or etch the surface. After washing off the residues clean the panels as described in 5.1. 5.3 Protection After Preparation--Use panels immediate!' after preparation or store wrapped in clean, hard surfaced paper to minimize lint on the glass surface. To avoid contamination by Fingerprints, do not touch the surface o the panels after preparation. Handle only by the edges. 6 Clack Vitrolile (Libby-Owens-Ford Glass Co.) and Carrara (PPG Industries) glass have been found satisfactory for this purpose and are obtainable from somi local glaziers. 586 DUP0502 97767 # D 3891 The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own respons/5/%. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapprovedor withdrawn. Your comments are Invited either for revision of this standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 587 DUP050297768 1 }' mm Designation: D 3911 - 89 Standard Test Method for Evaluating Coatings Used in Light-Water Nuclear Power Plants at Simulated Design Basis Accident (DBA) Conditions1 This standard is issued under the fixed designation D 3911; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parenlheses indicates the year of last reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. INTRODUCTION During a design basis accident (DBA) in nuclear power plants, conditions in the reactor containment will be characterized by elevated temperature and pressure, as well as the presence of a radiation environment. Water sprays, with or without chemical additives, may be used in the primary containment to suppress the consequences of the incident, to scavenge radioactive products, and to return the containment to near-ambient conditions. 1. Scope 1.1 This test method establishes procedures for evaluating protective coating systems test specimens under simulated DBA conditions. Included are a description of conditions and apparatus for temperature-pressure testing, conditions for radiation testing, and procedures for preparing, exam ining, and evaluating the samples. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 714 Test Method of Evaluating Degree of Blistering of Paints2 D 1193 Specification for Reagent Water3 4 D 4082 Test Method for Effects of Radiation on Coatings Used in Light-Water Nuclear Power Plants2 2.2 ANSI Standard:4 N512-1974 Protective Coatings (Paints) for the Nuclear Industry. 3. Terminology 3.1 Definitions: 3.1.1 blistering--the formation of bubbles in a coating (paint) film. 3.1.2 boiling water reactor (BWR)--a reactor in which the water moderator-coolant is boiled directly within the reactor 1 This method is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.02 on Service and Material Parameter. Current edition approved Feb. 24, 1989. Published April 1989. Originally published as D 3911 - 80. Last previous edition D 3911 - 80*5. 2 Annual Book ofASTM Standards, VoJ 06.0J. 3 Annual Book ofASTM Standards, Yols 06.03 and 11.01. 4 Available from American National Standards Institute, 13th Floor, II W. 42nd St., New York, NY 10036. core. The pressure in the reactor vessel is only slightly greater than the steam turbine pressure. 3.1.3 chemical spray--a solution of chemicals, such as those contained in Table 1, which could be used during a loss of coolant accident (LOCA) to suppress the incident, iscavenge fission products, and to return the facility to near-ambient conditions. 3.1.4 coating (paint) system--a polymeric protective film consisting of one or more coats applied in a predetermined order by prescribed methods to a defined substrate. 3.1.5 cracking---a break or a split in the coating (paint) system extending through the film or to the substrate. 3.1.6 curing--the transformation of a coating or other material into a solid phase or film. 3.1.7 DBA--a generic term for any one of a family of accident conditions which can result from postulated events. These conditions are generally associated with the rupture of high energy piping, The more commonly recognized acci dent conditions used to evaluate coating systems for priman containment are the LOCA or main steam pipe break. 3.1.8 deionized water--water prepared by an ion ex change process meeting the requirements of Specificatic D 1193, Types II and III. 3.1.9 delamination--separation of one coat or layer from another coat or layer, or from the substrate. 3.1.10 engineered safety system--a system designed 1o mitigate the effects of a design basis accident. 3.1.11 irradiation--exposure to ionizing radiation. 3.1.12 light-water nuclear reactor--an apparatus, using; light water as a moderator, in which fissionable material b arrayed so that controlled nuclear fission may be sustained in a self-supporting chain reaction. 3.1.13 LOCA--the specific conditions anticipated fol- TA8LE 1 Typical Spray Solutions Composition Chemical Compound Concentration (in Deionized Water) A Sodium borate Sodium hydroxide B Boric acid Hydrazine Sodium phosphate, dibasic 2000 to 4000 ppm boron adjust solution to pH 9.0 to 10.0 2000 to 4000 ppm boron 50 ppm unreacted excess adjust solution pH to 6.8 to 10.0 588 DUP05 02 97769 D 3911 ling a loss of coolant accident that would expose the ped surface of the containments of a light-water nuclear |er facility to the temperature-pressure environmental neters described. . 14 peeling--separation of one or more coats or layers i coating from the substrate. j.1.15 pressurized-water reactor (PWR)--a nuclear power or design utilizing liquid water under high pressure as erator-coolant. 1.16 quality assurance--the verification of the conform- of materials and methods of application to the govtig specifications, in order to achieve the desired result. i.17 reactor containment (containment)--the enclosure Sided to protect the environment from the consequences Inuclear incident. jgnlficance and Use Wi 1 This test method is designed to provide a uniform test .Jo determine the suitability of coatings used inside primary (Jhntuniment of light-water nuclear facilities under simulated conditions. Variations in actual surface preparation itJ in application and curing of the coating materials may Jdire additional testing as deemed necessary by the'speci al or qualifying agency, or both, if it is anticipated that the itions may adversely affect the performance of the pig system during a DBA. This test method is intended m o demonstrate that under DBA conditions, the coatings bjl remain intact and not become debris which could promise engineered safety systems; Ifeparatus ., ` 5.1 Environmental Test Chamber, constructed of mate'Ipit are cd'rrosion-resistant to the test solutions. \2 The equipment shall be capable of reproducing and (giBuously recording the temperature and pressure profiles t JgtiffiA conditions. C 3 \ sufficient number of thermocouples shall be located t life test chamber to assure conformity to the test curve, and so that both the temperature of the vapor phase and of the liquid phase (if present) can be recorded. 6. Preparation of Test Specimens 6.1 Determine the appearance of the test panels prior to testing by photo documentation or equivalent methods in order to provide a basis for post-test comparison. The testing requirements should indicate if this assessment will be done prior to shipping to the test facility. 6.2 Unless otherwise specified, a minimum of four sam ples shall be required to establish conformance of a given coating system on a given substrate, with two of the four samples being irradiated prior to testing in accordance with Test Method D 4082. Typical laboratory test panels are 2 by 4 by Vs in. for steel panels and 2 by 2 by 4 in. for concrete panels. 6.2.1 Steel Panels--Prepare in accordance with ANSI N5J.2 or as necessary to duplicate actual conditions. 6.2.2 Concrete Bloch--Prepare in accordance with ANSI N512 or as necessary to duplicate actual conditions. 7. Procedure 7.1 Test Parameters: 7.1.1 Test coatings using the applicable curves from the latest Safety Analysis Report (SAR) identified by the owner for Ihe specific containment. Illustrations of time-temperature-pressure test curves that simulate primary containment atmospheres during a DBA are shown in Figs, t and 2. 7i 1.2 The curves depicted in Figs. 1 or 2 may be used if they represent conditions equal to or more severe than those DBA'conditions anticipated. 7.1.3 The parameters of the curves may be simulated during testing as continuous functions or as an enveloping stepwise function. 7.1.4 Steam is used initially to achieve the desired thermal shock and to raise the test chamber and its environment to the prescribed test conditions. After equilibrium is achieved, the temperature of the test chamber is maintained by means FIG. 1 Typical Design Basis Accident (DBA) Testing Parameters (Temperalure-Time-Pressure)--BWR Dtywell 589 DUP050297770 D3911 TIME (SECONDS) FIG. 2 Typical Design Basis (DBA) Testing Parameters (Temperature-Time-Pressure)--PWR Containment of internal or external resistance, or both, heating elements, or other suitable means. The duration of steam injection should be minimized, as much as feasible, and the duration shall be recorded. Where inlet steam temperatures exceed 370F, initial steam injection shall be no longer then 15 min. 7.2 Spray Solution: 7.2.1 Unless otherwise specified, use deionized water when testing under simulated DBA conditions. 7.2.2 Record the chemical composition of the spray solution before each test. 8. Examination and Report 8.1 Examination: 8.1.1 Examine and evaluate test specimens within 4 h and again after 14 days following removal from the test chamber for the following coating defects: 8.1. J. 1 Delamination and peeling. 8.1.1.2 Cracking. 8.1.1.3 Blistering in accordance with Test Method D 714. 8.1.2 Unless otherwise instructed, disregard the condition of the edges and plane areas within `/i in. (6.4 mm) from the edges of the steeL or concrete test surfaces, and the top and bottom ends of the concrete surfaces. 8.2 Report--Report the following information: 8.2.1 The results of the evaluation of each test specimen. Report for all sides of concrete blocks and front and back of steel panels. 8.2.2 The extent ofeach defect from 8.1. Report "none" if po defects are present. 8.2.3 Any observations of unusual appearances.9 9. Acceptance Criteria 9.1 Peeling shall not be permitted. 9.2 Delamination shall not be permitted. 9.3 Cracking is not considered a Mure unless accompa nied by delamination or loss of adhesion. 9.4 Blisters shall be limited to intact blisters which are completely surrounded by sound coating bonded to thstj surface. 9.5 An owner may establish acceptance criteria more stringent than above. The above criteria are meant tn establish minimum standards only. 10. Documentation 10.1 Testing Procedures--Document each of the fol lowing: 10.1.1 A description of the test apparatus, temperature' and pressure profiles, spray solution composition inclining pH, duration, frequency, and rate of spray solutions, and any f other pertinent test conditions. 10.2 Test Agency: 10.2.1 The testing agency shall be responsible for Ihe documenting, reporting, and certifying of all tests. 10.2.2 The testing agency shall be responsible for meeting ' applicable quality assurance requirements. 10.2.3 The testing agency shall be responsible for pro- ` viding color photographic documentation of the test surfaces > as required. 10.2.3.1 Photographs shall reflect the actual size as close-* as possible of the test specimens. 11. Repairability 11.1 Test repair coatings applied to significant areas within Service Level 1 in accordance with the requirements for radiation and DBA conditions. 11.2 The test shall include evaluation of the repair coating applied in accordance with the repair procedure over the intended surface preparation or the original qualified coating system, or both. 11.3 Significant areas shall be determined by the speci fying or qualifying agency. Nonsignificant areas have been determined as being less than 2 ft2 in an approximate 2000 ft2 area; larger areas require a decision regarding significance 590 DUP050297771 (Precision f.l Test equipment must be demonstrated to have the ability to reproduce the design time/temperature params within 10 s and 5 F and the design pressure within 3 psig. In any test where the test equipment imposes variances in the pressure/temperature parameters that are outside this range, an analysis of the validity of these test results should accompany the test data. The American Society for Testing and Materials takes no position respecting the va/id/fy of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that deferm/naf/on of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be received every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for rev/s/on ofthis standard or for additionalstandards and should b$ addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 591 - .........------m DUP050297772 Designation: D 3912 - 80 {Reapproved 1989) Standard Test Method for Chemical Resistance of Coatings Used in Light-Water Nuclear Power Plants'* This standard is issued under the fixed designation D 3912; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the yeaT of last reapproval. A superscript epsilon (' ) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method establishes procedures for the evalu ation of the chemical resistance of coatings used in lightwater nuclear power plants. 1.2 This standard may involve hazardous materials, oper ations. and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D714 Test Method for Evaluating Degree of Blistering of Paints12 D 1193 Specification for Reagent Water3 2.2 MACE Standard: NACE TM-01-74 Laboratory Methods for the Evaluation of Protective Coatings Used as Lining Materials in Immersion Service4 2.3 ANSI Standard: N512-1974 Protective Coatings (Paints) for the Nuclear Industry, Section 75 3. Significance and Use 3.1 The specific chemical resistance tests to be performed are dependent upon the relative severity of the service conditions. Figure 1 should be used as a guide to chemical solutions commonly used in various types of facilities. These listed solutions should not be construed as all-inclusive. Specialized conditions may require chemicals or concentra tions not listed. In such cases, applicable solutions may be used. 3.2 The lining test may be used to evaluate the resistance characteristics of coating systems for lining surfaces of tanks, vessels and similar facilities used in a light-water nuclear power plant. 4. Preparation of Test Specimens 4.1 Steel Panels: 1 This test method is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.02 on Service and Material Parameters. Current edition approved May 30, 1980. Published July 1980. 2 Annual Book ufASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 4 Available from the National Association of Corrosion Engineers, P.O. Box 218340, Houston, TX 77218. s Available from American National Standards Institute, 13th Floor, 11 W. 42nd St., New York, NY 10036. 4.1.1 Prepare steel panels in accordance with ANSI N512.6 4.1.2 Use carbon steel panels in lining tests at least 7 by 7 by Va in. (178 by 178 by 6.4 mm) thick for Procedure A only. 4.2 Concrete Blocks--Prepare blocks in accordance with ANSI N512 with the exception that the top and bottom ends of the block shall be coated. 5. Sampling 5.1 Prepare individual specimens for testing in each of I pertinent solutions. 5.2 Prepare one additional specimen as a control. Mul tiple tests may be performed. 6. Procedure 6.1 Test in accordance with NACE TM-01-74, Procedure 1 B, Immersion Testing, except use Procedure A, One-Side Testing (cold wall) when a significant temperature differen tial is anticipated across the coating film as for tank linings. 6.2 Lining Test: 6.2.1 Immerse lining test specimens in the appropriate test solutions listed in Fig. 1 or as otherwise specified for a minimum of 180 days. 6.2.2 Maintain a temperature of 72 5F (22 3 C) unless otherwise specified by the purchaser. 6.2.3 Use deionized water with an initial resistivity of not less than 1 MQ/cm at 77F and with a total solids of mm. than 0.5 ppm, more than 0.15 ppm of chloride or more th 0.15 ppm of fluoride. Maintain the pH range from 6.0 to 8.0. ' 6.2.4 Change the deionized water daily during the fir>t week and weekly thereafter. Measure any constituents leached out before the water is changed. 6.3 Chemical Exposure Tests: 6.3.1 Test the chemical resistance properties of the < ings by immersion in the appropriate test solutions listed in Fig. 1 or as otherwise specified for a time interval that str.ll vary as follows. 6.3.1.1 For simulated exposure to occasional splash and spillage on areas where the solution may evaporate in pla e immerse the specimens for a period of 5 days in the listed reagent solutions. 6.3.1.2 For simulated exposure to decontamination solu tions, immerse the specimens for a period of 24 h in the listed solutions. 6.3.1.3 For simulated exposures to corrosive fumes of the listed reagents, immerse the specimens for a period of 8 h. 6 An ASTM standard will be published in the future and will replace threference to ANSI N512 in this standard. 592 lecirr atiri| DUP050297773 # D 3912 fcimen Mo.. Sling System: Primer . Intermediate . Finish ____ CHEMICAL-EXPOSURE TEST RESULTS OFT DFT DFT ) Numbers) _ Method of Application _ eF, Relative Humidty___ %, Curing Time- fcl jrfoce Preparation n 'iy. ith' ids; |J "V 1 Chemical Sera/ Service. Idrazine (NH2NH2) Ifliurn borate (Na^cy <n' 20) lionized water ||dium hydroxide (NaOH) htaminatton Solutions: gjfc acid (CaHe0,-H2O) Sum phosphate dibasic (Na^HPO*) Jlfogen peroxide (f*fed2) jftasslum permanganate (KMnO*) `Slum fluoride (MaF) idlum thiosulfate (NagS203 *5H20) j, I medium'phosphate (Na3P04*12H20) Concentration, weight % 5 5 5 5 1.03 4.6 2 ' 2' 11.5 24 h 5 days At n-s te | FIG. 1 Sample Form 4'll 3,2 Maintain a temperature of 72 . 5F (22 to 3"C) nless the service conditions require a higher temperature. 3.3 Use reagent grade chemicals and distilled wafer forming to Specification D 1193, Type III, for all solu tions. pfexamination and Evaluation 7.2 Chemical Exposure Tests: 7.2.1 Examine the test specimens at the end of the test period or every 24 h, -whichever is the shorter time. 7.2.2 Evaluate the condition of the specimens within 1 h after removal from the test solutions. 7.2.3 Evaluate the test specimens at each inspection as in 7.1.3. ia " n !-* |;1 Lining Test: I:. 1.1 Examine the test specimens weekly for the first Mth and then monthly thereafter. p.1.2 Inspect specimens immediately upon completion of 8. Documentation and Report 8.1 Report all procedures and conditions relating to the test specimen preparation. 8.2 Document the testing procedure and test results. A |ge test period. Make a final inspection not later than 24 h suggested format is illustrated by Fig. 1. Jailer removal from the test solution. 1.3 Evaluate the test specimens at each inspection for Hiding, delamination, blistering (Test Method D 714), dis- ki |.Coloiation, and softening. 9. Precision and Bias 9.1 These tests are qualitative in nature. Precision and bias are not definable. IF I M The American Society ter Testing end Materials takes no position respecting the vatdily o! any patent rights asserted In connection with any Item mentioned in this stsndsrd. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibly. 'a This standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if not rewsed, either reapprovsd or withdrawn. Your comments are Invited either for revision of this standard or tor additional standards and shoutd be addressed to ASTM Headquarters. Your comments wttt receive careful consideration et a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race SI., Philadelphia, PA 19103, f* 593 DUP050297774 Designation: D 3924 - 80 (Reapproved 1991)* Standard Specification for Standard Environment for Conditioning and Testing Paint, Varnish, Lacquer, and Related Materials1 This standard is issued under the fixed designation D 3924; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearoflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. il Nop' --Keywords were added editorially in January 1991. 1. Scope 1.1 This specification defines the standard atmospheres for normal conditioning and testing of paint, varnish, lacquer, and related materials, at approximately ambient conditions. Nqr' 1--See Definitions E41, Specification E 171 and Method E337. 2. Referenced Documents 2.1 ASTM Standards: E 41 Definitions of Terms Relating to Conditioning12 E 171 Specification for Standard Atmospheres for Condi tioning and Testing Materials3 E 337 Test Method for Measuring Humidity with a Psychrometer (The Measurement of Wet- and Dry-Bulb Temperatures)4 3. Standard Atmosphere 3.1 Unless otherwise specified, conditioning and testing of coating materials known to be sensitive to variations in temperature or relative humidity shall be carried out in an atmosphere having a temperature of 73.5 3.5F (23 2C) and a relative humidity of 50 5 %. If closer tolerances are 1This specification is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO1.20 on Quality Assurance and Statistics. Current edition approved Sept. 2, 1980. Published November 1980. 1 Annual Book ofASTM Standards, Vol 14.02. 3 Annual BookofASTM Standards, Vol 15.09. 'Annual Book ofASTM Standards, Vol 11.03 and 15.09. required, 2F ( 1 C) or even narrower limits, and 2 % relative humidity may be specified. 3.2 The standard room or cabinet shall be well-ventilated but free of drafts, dust, products of combustion, and labora tory fumes. Lighting conditions, unless otherwise specified shall be that normally maintained in a room used for paint1 test purposes. 4. Standard Temperature 4.1 Unless otherwise specified, the standard test temperature shall be as specified in Section 3. 5. Room Temperature 5.1 A temperature in the range from 65 to 85"F (18 to 29.5C) shall be called room temperature. 6. Conditioning and Testing 6.1 Unless otherwise specified in the test method, condi tion the organic coating materials or dried test films thereof and the test equipment for not less than 3 h in the appropriate atmosphere and verify the temperature of the material before conducting the test in the same atmosphere. 6.2 For routine testing where close temperature control is' not critical, conduct all physical tests on organic coating materials or dried test films thereof at the room temperature of 65 to 85"F (18 to 29.5C). 6.3 For referee testing, unless otherwise specified in;tjt"! test method, conduct all physical tests on organic coating " materials or dried test films thereof in the standard aumisphere as specified in Section 3. 7. Keyword 7.1 conditioning environment The American Society for Testing amt Materials takes no position respecting the validity ot any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, end the risk of Infringement of suoh rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either torrevision ofthis standard ortor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may altemf. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards,. 7916 Race St., Philadelphia, PA 79103. 594 DUP050297775 Designation: D 3925 - 91 Standard Practice for Sampling Liquid Paints and Related Pigmented Coatings*1 This standard is issued under the fixed designation D 3925; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (' ) indicates an editorial change since the last revision or reapproval. -2 '.c tilatcd abo"aciheri, paint -ricope Bs' This practice describes methods of taking representa|isamples of fluid paint or pigmented coating products , i containers of any type. ffaT 1,1 The sampling of dry powder paints, clear coatings, iScd solvents, and nonpigmented materials of any type is jH'gpt covered in this procedure. . \} This standard does not purport to address all of the >' fyvafetv problems, if any, associated with its use. It is the i'^isfonsibility of the user of this standard to establish appro- V'prwfe safety and health practices and determine the applicaWm ofregulatory limitations prior to use. ipeialts to PY** Kuferenced Document HI.1 ASTM Standard: VO 1475 Test Method for Density of Paint, Varnish, Lacte A quer, and Related Products2 it *he ating juos- jjerminology HI Description of Term Specific to This Standard: ijl. l batch--the quantity of liquid paint or coating pro||Id in the final mixing operation after all production jgesses are complete. For example, when a number of pent dispersions are reduced with additional vehicle jpther in a large tank, the resulting final mixture is one Hbh. ' isSr'1 p4. Significance and Use 4 I Samples are taken from batches, lots, and shipments Isfccf p unt in order to determine their uniformity and compli'lj&4iKC with specification requirement?. It is very important " jffhat these samples be of convenient and economical size and ^ffitthey be representative of the batch ofpaint at the time it gg| filled into shipping or storage containers. B,2 The time and effort necessary to ensure that the title is representative of the original material will be Jpfid in reduction of laboratory work and elimination of wjsible rejections of acceptable material. | Sampling Considerations 19.1 The use of common sense and good judgment is Pjnportant even in the apparently simple task of taking pimples. This practice is under the jurisdiction of ASTM Committee D-1 on Paint and plated Coatings and Materials and is the direct responsibility of Subcommittee 1.20 on Quality Assurance and Statistics. i Current edition approved Sept. 15, 1991. Published November 1991. Origi- ijjly published as D 3925 - 80. Last previous edition D 3925 - 81 (1985)C1. P Annual Book ofASTM Standards, Vol 06.01. 5.2 Use care to assure that all containers, agitating equip ment, and sampling apparatus are clean and that they can in no way contaminate the sample being taken. Slight contam ination of the paint sample may lead to false test results. 5.3 The sample container should be dry and not cooler than the temperature ofthe area in which the sample is to be taken. 5.4 Because pigmented coatings are dispersions and not solutions, finely divided pigment particles dispersed in the coating vehicle may settle upon standing. Consequently, thorough and careful agitation before sampling is necessary to restore the paint to its original, uniform condition. The method of agitating or stirring is therefore of prime impor tance. 5.5 As soon as samples of paint are taken from the shipping or storage container, place them in clean, nonreactive, dry, air-tight containers to prevent evaporation. Do not store samples in plastic bottles because volatile solvents may diffuse through the walls. Loss of volatile solvents may introduce errors in such tests as viscosity, weight per gallon, and nonvolatile content as well as other properties. If cap liners are used, they should also be nonreactive with the material. If the sample is self reactive or highly volatile, appropriate sample container precautions should be taken to prevent over-pressurization of the con tainer. 5.6 When representative samples have been obtained and packaged in clean, closed containers, deliver them promptly to the testing laboratory. During the period between sam pling and delivery to the testing laboratory it is important that samples be kept at temperatures from 40 to 100"F (5 to 40Q because extremes of temperature may change proper ties of some paint products. 6. Procedure 6.1 Because of differences in physical properties, some what different procedures are required for agitating and sampling those paints containing water as the volatile component in comparison to those containing organic sol vents. For coatings with no volatile ingredients, use the method'applicable to materials containing organic solvents. 6.2 Pigmented Coatings Containing Organic Solvents-- Materials in this group are of many different types but all contain organic solvents, not water, as their volatile portion and they are fluids, not dry powders. 6.2.1 Small Containers: 6.2.1.1 When the batch to be sampled is filled in small containers and batch numbers are marked on the container, put all containers from the same batch together. From each batch select at random 1 % of, but not more than five containers, using the next larger whole number if a fraction 595 DU P050297776 D 3925 results. For example, if there are 275 containers in a batch, select three for test. 6.2.1.2 After selection of the filled, unopened containers, thoroughly agitate or stir the contents by the best means available. Acceptable methods of mixing are mechanical shaking or stirring or hand stirring with a paddle, followed by "boxing," that is pouring back and forth between the original and a clean empty container. Mechanical shakers are desir able for most materials since there is thorough agitation in a closed container. To prevent evaporation, agitate in a closed container lacquers and other coatings containing a highly volatile solvent. 6.2.1.3 Before mechanical shaking, open the container and check to be sure that the pigment has not caked on the bottom of the container. If this condition exists, stir manu ally to break up the hard settling and then put the containers on the mechanical shaker. Agitate paints having a weight per gallon of 11 lb (1.3 g/mL) or less on the shaker for 10 min and those with a weight per gallon of more than 11 lb for 20 min. 6.2.1.4 Once the contents have been thoroughly agitated, pour half of the material into an empty container and take a 1 qt (1 L) (or smaller iftaken from a container of 1 qt or less) sample from each half. Determine the weight per gallon on each sample in accordance with Test Method D 1475. The two determinations should not differ more than 0.5 %. If the results differ by more than this the paint is not thoroughly mixed. Return the material to the original container, stir again, and repeat the test. 6.2.2 Containers Larger than 5 Gal: 6.2.2.1 30 and 55-Gal Drums--From each batch select at random 5 % of but not more than three containers. Drums may be stirred satisfactorily by several; means. With openhead types, mechanical or manual stirring may be used. Some drums contain their own agitators; drum shakers or rollers may also be used. After thorough agitation, take samples from the top and bottom of the drum and compare weights per gallon as described in 6.2.1.4. 6.2.2.2 250 to 500-Gal Containers (Tote Tonics)--Select at random 25 % of all containers for test. Take samples from top and bottom of the container and compare weight pcr gallon determinations as described in 6.2.1.4. 6.2.2.3 Tank Wagons and Tank Caw--Sample each com partment of the wagon or car. Pigmented paints and coatings packaged in large containers are generally formulated to be essentially nonsettling. Therefore, take samples from the top, middle, and bottom of the container and make weightper-gallon determinations before any vigorous stirring is done. If the resulting tests fall within the limits describe! earlier, no further agitation is necessary. Samples may bi obtained with a Bacon-bomb sampler or a "thief" apparatus 6.3 Pigmented Coatings Containing Water: 6.3.1 Handle pigmented coatings containing water (latex paints, etc.) in a slightly different manner from solventthinned coatings. Water-thinned paints, if stirred too vigor ously, have a tendency to incorporate air bubbles, whiol sometimes result in changing the physical properties of thi paint. 6.3.2 With the above consideration, take the samples in accordance with the same general procedure outlined in 6.2 for paints containing organic soLvents. If it has been neces sary to shake, stir, or agitate a water-thinned paint vigor ously, deaerate the samples before the weight-per-gallon test! are run. 6.4 Samplingfrom Tanks at the Factory--Mix the mate rial in the tank thoroughly before completely filling two 1-qi (1-L) containers. If the containers are to be filled from? valve on the bottom or side of the tank, mix the material draw off at least 5 gal (20 L) through the valve and ret '-ri ti the tank before taking the sample. 6.5 Sampling During Filling of Containers at the Fac tory-kites the material is thoroughly mixed in the ta 1 filling ofcontainers has commenced, take a I-qt (1-L) sample when about 25 gal (100 L) have been filled and another wh ,i . about 25 gal remain to be filled. 7. Keyword 7.1 sampling The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, (f you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St,, Philadelphia, PA 19103. -a 596 DUP050297777 Designation: D 3927 - 87 Standard Guide for State and Institutional Purchasing of Paint1 Ks* This standard is issued under the fixed designation D 3927; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. The committee responsiblefor this standard has voted its withdrawal. In the absence ofsubstantial reasons that it should be continued, !:!* O-flB. 'Scope the Society will approve withdrawalfrom publication in February 1993. D 2197 Test Method for Adhesion of Organic Coatings by This guide aids state and local governments to make meal decisions in purchasing architectural paints on the pS of both quality and cost. P This guide concerns itself primarily with architectural Up'Sales paints as listed in Annex A2.2 especially whites tints. Emphasis on this group of products is justified by If preeminence in usage and the difficulty in describing in lie terms requirements applicable to them. g|OT 1--With experience much of the logic and many of the piques described herein can be found applicable to a broad range of ijMgiteural coatings. B Many different methods can be used to select coatings. jg|? methods are presented in this guide and the user may Scrape Adhesion2 D2243 Test Method for Freeze-Thaw Resistance of Wa ter-Borne Paints2 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates2 D2366 Test Method for Accelerated Testing of Moisture Blister Resistance of Exterior House Paints on Wood3 D 2486 Test Method for Scrub Resistance ofInterior Latex Flat Wall Paints2 D2805 Test Method for Hiding Power of Paints by Reflectometry2 D 3258 Test Method for Porosity of Paint Films2 D3359 Test Methods for Measuring Adhesion by Tape Test2 flpp the method or combination of methods best suited to J&eds. The three methods are: D3719 Test Method for Quantifying Dirt Collection on Coated Exterior Panels2 Sections D3928 Test Method for Evaluation of Gloss or Sheen M ^^iflngredients/Cost Ratio Method WStrnance/Cost Ratio Method ^jpleation Method 4 Uniformity2 5 D 4062 Test Method for Leveling ofPaints by Draw-Down 6 Method2 HCferenced Documents Jp j ASTM Standards: D4400 Test Method for Sag Resistance of Paints Using a Multinotch Applicator2 T|pj44 Test Method for Relative Hiding Power ofPaints by jH r_ |jjtjie Visual Evaluation of Brushouts2 m D 523 Test Method for Specular Gloss2 . l|j|.f>2 Test Method for Consistency of Paints Using the IgStormer Viscometer2 59 Method of Evaluating Degree of Chalking of (.Exterior Paints2 660 Test Method for Evaluating Degree of Checking of Exterior Paints2, '" 4.-D661 Jest Method for Evaluating Degree of Cracking of S'f Exterior Paints2 n Pjj|f>662 Test Method for Evaluating Degree of Erosion of Exterior Paints2 ^ D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints2 l' D 1475 Test Method for Density of Paint, Varnish, Lac- quer, and Related Products2 ^ 171640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature2 This guide is under the jurisdiction of ASTM Committee D-l on Paint and Plated Coatings and Materials and is the direct responsibility of Subcommittee l||P 1.41 on Government Procurement Criteria for Commercial Paint and Coatings. C nrent edition approved Aug. 28, 1987. Published October 1987. Originally JjpbTished as D 3927 - 80. Last previous edition D 3927 - 80. 2 Annual Book ofASTM Standards, Vol 06.01. 3. Products 3.1 It is recommended that standard commercial products offered to the general public for a period of 2 years or produced and sold in accordance with applicable govern ment specifications be considered for purchase by the methods described in Sections 4, 5, or 6. 4. Active Ingredients/Cost Ratio Method 4.1 This method utilizes, as an indication of quality, the coating composition provided by the manufacturer and is limited to interior and exterior wall paints listed in Annex A2.2. 4.2 Only those ingredients considered to contribute di rectly to quality are considered. The major active ingredients in most paints arc vehicle solids/ or binder and primary hiding pigments. 4.2.1 The weight percent of vehicle solids may help to predict the scrubbability or cleanability of a paint, but the quantity of pigment must also be considered. In general, the greater the ratio of vehicle solids to pigment, the better the scrubbability and cleanability will be. The ratio of vehicle solids volume to pigment volume is a more useful parameter 3 Discontinued; see 1988 Annual Book ofASTM Standards, Vol O6.0i. dill 597 DU P050297778 but is not readily available. Moreover, each type of vehicle solids, such as alkyd in solvent-borne paints and vinyl or acrylic latex in waterborne paints, has its own properties and there are many other additives not shown that can affect scrubbability, cleanability, and other properties. 4.2.2 The amount of primary hiding pigment, for ex ample, titanium dioxide in a white or pastel gloss finish, is an indication of hiding power. Paints of equal depth of color (light reflectance) should be compared, since lightness affects visual hiding. 4.3 An advantage of the method is that no special equipment or experience is required. Even if extensive testing is possible, the active ingredients/cost ratio method is valuable for initial screening. The active ingredients/cost ratio for several types of paint can be combined into a single figure for each supplier with each paint's "Use Factor." (see Section 7 and Annex A5). 4.4 The active ingredients/cost ratio method is not as conclusive for flat paints that often have a high "Use Factor." The hiding (opacity) of flat paints, particularly latex paints, cannot be predicted from the amount of hiding pigments since these paints often obtain much of their hiding from air in a porous paint film (conventional dry hiding) or air incorporated in the components of the film (micro-void techniques). Consequently, performance tests should be made on latex flat paints whenever possible. The cost per gallon of those latex flat paints with acceptable performance can be used in conjunction with the active ingredients/cost ratio for this type of paint. 4.5 Calculation ofIngredients/Cost Ratio--Use the proce dure in Annex A1 to calculate the ratio of active ingredients to unit cost of the paint. The greater the ratio, the more active ingredients a paint has per unit cost. In general, this will help determine if a paint is a good buy for the money, but may not determine the quality of a paint. Nst' 2--A lower quality paint at o lower cost may tie a good buy, but may not be of the desired quality. 5. Performance/Cost Ratio Method 5.1 Paint can be tested using standard test methods such as those suggested in Annex A2. Although there are many other test methods used in paint formulating and manufac ture, the methods listed have been found to be most useful to the consumer in determining the quality of a product. 5.2 Since different products have different properties, specific test methods have been suggested for each type of product shown in Annex A2. The purchaser may eliminate some of these tests, if the property that the test measures is not important to him, or may add other tests. 5.3 Paint testing by the purchaser requires purchase oftest equipment and some skill in performing and interpreting test results. However, a few basic tests such as hiding (opacity), porosity, or scrubbability can be tun with relatively inexpen sive equipment and will help considerably in determining the quality of a paint. 5.4 The quality of a paint can be determined by analysis of test results. Some results are descriptive, such as "good" or "poor" while others are numerical but with large numbers from some test methods, such as 450 for scrubbability, or small numbers from others, such as 0.990 in measuring hiding. Also with some tests the higher the numerical values, the better the quality, but with others lower values indicate better quality. For these reasons the original results from the different tests cannot be directly combined into an equation to provide a numerical ranking. 5.5 If the purchaser wants a numerical value for overall quality to use in ranking various products, it is suggested that a scale from 0 to 10 be used for all test methods. Descriptive words can be converted to a numerical rating scale such as: Excellent Very good Good Fair Poor Very poor Many ASTM test methods already use the 0 to 10 scale, but numerical results can be converted to this scale as shown in ' Annex A3. No t e 3--ASTM does not intend to define quality for the purchaser, The scales shown in Annex A3 are given as examples that can be,! modified by the purchaser, if desired. 5.6 Many of the important properties of a paint that ca| be tested and evaluated by a professional painter are listed it) J Annex A2. The purchaser can request that the painter note | unusual behavior during the application ofthe coating; *=i'ch .< judgemental rating of properties not normally tested cat. be 1 used as an aid in the paint selection process. 5.7 Calculation ofPerformance/Cost Ratio: 5.7.1 Use the procedure in Annex A4 to calculate tb$3 performance/cost ratio from the results obtained from lab#F ratory tests or those supplied by painters, or both. ? 5.7.2 The calculated ratio will indicate if a paint has high, j performance relative to cost. It is possible to have a highJj relative ratio even though the overall quality may be low irf the paint is low in cost. The overall quality of producM should, therefore, enter into cost comparisons to ensure thaw they provide the quality desired by the purchaser. It is aljffijj possible to have a high overall quality rating for a paint an(nl still have some property that is not acceptable to purchaser. It is therefore suggested that minimum stin v ,! be established by the purchaser for those proper i; considers important. 5.8 Information Provided by the Supplier--If the pur-'f| chaser is not equipped to perform tests, he can request fijgf manufacturer to supply test results that can be used fiffij performance/cost evaluations. Ifthe purchaser is equipped to, run some simple tests or ifa professional painter is availaliif for evaluation, he need ask the manufacturer to supply da*1 only for those properties requiring considerable skill :: expensive equipment to measure. 6.Specification Method 6.1 Specifications can provide a useful, mutually satisiacH tory mechanism for listing essential quality requirements ofa| product. A specification is a document that attempts ter* describe precisely the requirements that a product must meet; to be considered suitable for a particular use. Requireme it^ may be based on composition of the product or its perfor mance. Composition requirements are easier to iftoitiw*-. while performance requirements, which are preferred, ate; more difficult to establish and evaluate. Consequently, most coating specifications are a combination of both types. 598 DUP050297779 D 3927 iS Specifications establish the minimum level for a duct, but if requirements are set too low it becomes limit to purchase superior coatings that may be a better fe. Specifications may encourage manufacturers to for||fe special products that meet the specification but are ent from those sold to the general public. J3 State and local government purchasers may write a fefication for each product, but considerable knowledge uJpaint properties and how they are related to practical ' g^iilicat'on and performance of the product is required. X'^jCveirment purchasers may use Federal specifications ali? i ready prepared for many products. ! ,`tV. &:pUse Factor ? A use factor can be determined by dividing the total ! annual cost or quantity of each type of paint by the total cost or quantity of all paints used by the purchaser. These factors permit each type of paint to influence the evaluation of bids in direct proportion to the quantity used. 7.2 If a purchaser wishes to consider the purchase of a complete line of paint from one supplier, then all of the ingredient/cost or performance/cost ratios for each of the supplier's products can be averaged to give an overall value for each supplier's line of products. Since different products in a line may vary in quality, more emphasis should be given to those that the purchaser intends to use the most. This can be done by multiplying the ratio for each paint by the use factor as shown in Annex A5 to determine the weighted average. ANNEXES Al. CALCULATION OF INGREDIENT/COST RATIO 1.1 Obtain from the supplier the weight per gallon of the (Slit or take the weight per gallon in accordance with Test Mfthod D 1475. Id .2 Obtain the weight percent of active ingredients from Ijgisupplier. ipl.3 The relative hiding efficiency of the most common jvfite hiding pigments are as follows: Ifey. Efficiency Factor titanium dioxide %ft6|ase titanium dioxide 1.00 0.75 Efficiency Factor Lithopone Zinc oxide 0.18 0.14 Consider all grades of high content rutile titanium dioxide as 100 % active pigment even though the actual percent of titanium dioxide in the pigment is less than 100 %, since the total pigment contributes to hiding efficiency. Al .4 Example ofCalculations: Three latex paints A, B, and C are being considered for purchase AS i 1> Ingredients'1 idU&t' ggg^hniiim dioxide (83 % Ti02) ipium dioxide (90 % Ti02) tflhopone jieates fffgium carbonate ||lhyl-acrylic resin solids lithihives Htfer Composition Weight, % ABC 17 13 L6 5 13 10 20 99 8 13 13 9 22 2 46 46 47 Weight/ga! ABC 11.54 11.50 11.00 (for all ingredients) Active Ingredient, lb/gal A BC 1.96 1.43 1.84 . 0.58 1.50 1.50 0.99 Hiding Pigment Efficiency Factor Active Hiding Pigments Vehicle Solids Total Active Ingredients/ Gal Cost/gal Ingredients/Cost Ratio 1.96 X 1.00 1.96 + 1.50 - 3.46 / 5.00 0.69 1.84 X 1.00 = 1.84 + 1.50 - 3.44 / 7.00 = 0.49 0.58 X 0.18 = 0.10 1.43 X 1.00 = 1.43 + 0.99 * - 2.42 / 3.40 = 0.71 Paints A and B both have about the same amount of active ingredients, but the cost oFB is higher. Paint B may have acceptable quality but it could be eliminated scause of cost. Paints A and C both appear to be good buys, but C with its lower amount of active ingredients may have a lower quality than A and some performance tests would be "rmmended. 1 Chemical tests may be run to confirm the accuracy of composition presented by the manufacturer. *1.1 il 5d ' !n i p* | 599 DUP0502 97780 # D 3927 A2. RECOMMENDED TEST METHODS Property Adhesion of organic coatings Adhesion by tape test Brush application characteristics Blister resistance--accelerated testing of moisture blister resistance ofexterior house paints on wood talking ofexterior paints Checking ofexterior paints Color compatibility Color difference of opaque materials Condition in container Consistency of paints using the stormer viscometer Cracking ofexterior paints Dirt pick-up Drying, curing, or film formation of organic coatings at room temperature Erosion of exterior paints Flaking (scaling) of exterior paints How properties Freeze-thaw resistance of latex and emulsion paints Gloss---specular gloss Hiding power of paints Hiding power, practical Hiding power--relative dry hiding power of paints Leveling characteristics of paint by draw-down method Porosity of paint films s Scrub resistance of interior latex fiat wall paints Sag resistance of paints using a multinotch applicator Stain removal Uniformity of gloss or sheen A2.1 These tests may be performed at the discretion ofthe purchaser to ensure satisfactory performance. A2.2 Types ofPaint: A Interior latex flat B Interior latex gloss and semigloss C Interior solvent gloss and semigloss D Exterior latex gloss and flat E Exterior solvent-borne gloss and flat Test Method D 2197 D33S9 painter D 2366 D $$$ q 530 in preparation & 2244 painter 0 562 D66I D3719 " 1640 0 gg2 p 772 painter jy 2243 p 523 0 2^3 painter . 0 344 0 4062 D32S8 0 2486 0 44q q in preparation 0 392$ 600 DUP050297781 # D 3927 A3. SUGGESTED 0 TO 10 SCALES FOB METHODS NOT ALREADY USING THIS SCALE* D 3258 Porosity (Percent Refleclance Drop) 1.000 0.995 to 0.999 0.990 to 0.994 0.985 to 0.994 0.980 to 0.984 0.975 to 0.979 0.970 to 0.974 0.965 to 0.969 0.960 to 0.964 0.955 to 0.959 0.950 to 0.954 10 9 8 7 6 5 4 3 2 I 0 to 4 5 to 9 10 to 14 15 to 19 20 to 24 25 to 29 30 to 34 35 to 39 40 to 44 45 to 49 50 to over D 2486 Scrubability Hat" 400 or over Gloss or Semigloss (Wall Paints) 1500 or over Flat Gloss or Sanigloss (Wall Paints) 9 360 to 399 1350 to 1499 8 320 to 359 1200 to 1349 7 280 to 319 1050 to 1199 6 240 to 279 900 to 1049 5 200 to 239 750 to 899 4 160 to 199 600 to 749 3 120 to 159 450 to 599 2 80to 119 ` 300 to 449 1 79 to 40 150 to 299 0 Oto 39 Oto 149 A The purchaser may wish to include a control material when paints are evaluated ora series ofpaints could be ranked to allow for variations In test methods or subjective evaluations. B See Footnote 5. A4. PERFORMANCE/COST RATIO I Three latex, flat wall paints A, B and C being dered for purchase are tested for the four listed properith the following results: 19--Hiding, Test Method D 2805 3--Brush Application, Painter : 23--Porosity, Test Method D 3258 124--Scrubbability, Test Method D 2486 Paint A 75 6.0 $8.50 Overall rating (mean) Cost per gallon Performance/cost ratio 6.0 $7.50 0.80 Paint C Rating Overall rating (mean) Cost per gallon Performance/cost ratio 96 5.5 $6.85 0.8O A4.2 Paints A and B'have the same overall performance rating, but paint A could be rejected because of its higher cost. Paints B and C have the same performance/cost ratio so they are both equal buys for the money. The purchaser, however, could decide that the value of 2 for the porosity of paint C is below his acceptable requirements for this prop erty and reject this paint. 601 DUP0502 97782 # D 3927 AS. USE FACTOR A5.1 Paints from two different suppliers being considered for purchase are evaluated according to the active ingre dients/cost ratio method with the following results: Paint Type A B C D E mean A B C D E mean A Ingredients/Cost Ratio 0.71 0.69 0.70 0.65 0.49 0.648 0.65 0.49 0.69 0.70 0.71 0.648 Supplier 1 Use Factor X 42.7 % X 24.0% X 15.0% X 10.0% X 8.3 % Supplier 2 X 42.7% X 24;0 % X 15.0% X 10.0% X 8.3% = = = Total = = = Total Weighted Ratio 0.30 0.17 0.10 0.07 0.04 0.68 0.28 0.12 0.10 0.07 0.06 0.63 1 Calculated from Annex AI. A5.2 The ingredients/cost ratios of each supplier's line of paints averaged the same (0.648), but when these ratios are weighted according to a use factor, then supplier No. 1 is.the better choice since paints with the better ingredient/cost ratios are the ones most used by the pin-chaser. However, testing is the key to assurance of obtaining an accept: product. A5.3 A use factor can also be used to weigh paint ,|i evaluated by the performance/cost method. The American Society tor Testing end Materials takas no position raspacting the validity ot anypatent tights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such pstent rights, and the risk of. infringement ot such rights, are entirely their own responsibility. This standard is subject to revision at any time by the respons/bte technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If, you feel that ypur comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. g.rute 602 DUPO 50297783 Designation: D 3928 - 89 Standard Test Method for Evaluation of Gloss or Sheen Uniformity1 This standard is issued under the fixed designation D 3928; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon U) indicates an editorial change since the last revision or reapproval. ! 1 This test method covers the determination of the ' &.;mty of gloss or sheen of a paint applied by brush to a panel simulating an interior wall section. Variations in ujpg or sheen that may be caused by short wet edge time, g|r leveling, and pigment orientation or flotation during Bafter application are evaluated visually, Jjf.2 Because both the application and the panel evaluation m-very subjective, this test method should be used only for Hparative testing within one laboratory as the ratings fggned by different laboratories do not usually agree (see jUii MIBbS This standard may involve hazardous materials, oper- and equipment This standard does not purport to fjMg-ess all ofthe safety problems associated with its use. It is \fflkresponsibility of the user of this standard to establish Jmdpriate safety and health practices and determine the Wmicability Ofregulatory limitations prior to use. Kshimmarv of Test Method K. 1 Paint is brush applied to a test panel using procedures ^conditions that are most likely to cause nonuniformity if gloss or sheen. The dry film is then viewed under >n<litions that accentuate variations in gloss or sheen and - --me overall appearance is evaluated. p{:Significance and Use J*3.1 When coatings are applied to large flat surfaces such ue. as walls, the film thickness may vary or there may be small ~ ivs missed entirely (holidays) when the color of the fresh J pttbrial and the previous film are very similar. It is much Ss costly if these areas can be touched up instead of having ;iJKo repaint the entire surface. 1.2 Thickness is also affected in the locations where an >t;.ncu coated a short time before is joined with the area jiSYui rently being coated (laps). An application technique that may affect the final appearance of the film is brushing or Polling the material in different directions in adjacent areas, Wfc 3.3 Both buyers and sellers are interested in determining ffjl'.vhether a coating can be applied without exhibiting areas j*.:h;it differ in appearance because of laps and brush or roller 1 Ifmarks, and whether it can be readily touched up to provide a r jpiniform appearance in regard to gloss or sheen and all other ^aspc cts. 1 This method is under the jursidiction of ASTM Committee EM on Paint and |^.elated Coatings and Materials and is the direct responsibility of Subcommittee I&0I.42 on Architectural Finishes. ___ Current edition approved April 14, 1989. Published June 1989. Originally " ^published as D 3928 - 80. Last previous edition D 3928 -80 (1987). 4. Apparatus 4.1 Paint Brush,1 2 in. (50 mm) wide with polyester bristles 2% in. (70 mm) long, chisel tip Vis in. (10 mm) thick. Previously used brushes are preferred. 4.2 Paint Brush* 1 in. (25 mm) wide with polyester bristles 2`A in. (57 mm) long, chisel tip Vie in. (15 mm) thick. Previously used brushes are preferred. 5. Reagents and Materials 5.1 Laminated Fiber Board,4 524 by 12 in. (610 by 300 mm) with at least one smooth side. 5.2 Latex-Base Primer* 5.3 Control Paint (optional)--Since there are no standard panels, photographs, or paints for this test method, an agreed-upon paint of known uniformity of appearance should be included with the test paints as a control, unless the paints are only ranked. 6. Procedure 6.1 Apply the latex primer by spray to the entire face of a smooth side of the test panel so as to coat it uniformly at a spreading rale of about 450 ft2/3gal (11 m2/L). 6.2 Air dry at least 18 h under standard conditions of 73.5 3.5F (23 2C) and 50 .5 % relative humidity and examine tlje panel for uniformity of primer application. If this appears satisfactory, divide.the coated area into sections A and B as shown in Fig. 1. 6.3 Mount the panel vertically and position it as shown in Fig. I'with section A to the right and section B to the left of the operator. Before painting, wet the brush with water if latex paints are to be tested or VM & P naphtha if the test paints are solvent reducible and shake out as much liquid as possible before using. Apply the paint under test to section A with the 2-in. (50-mm) brush (Note) at a spreading rate of 450 25 ft2/gal (11 0.5 m2/L). About 13 g are required to cover this area but theexact amount can be determined from the following equation: g = [Mx BO/S] x 3.15 where: A - area, in.2, W. = weight per gallon, lb/gal, and S = spreading rate, ft2/gal, 2 A polyester brush No. B-20CS from The Lencta Co., Ho-Ho-Kus, NJ, has been found suitable for this purpose. 3 A polyester brush No. B-10 from The Leneta Co. has been found suitable for this purpose. 4 Upson board, available from General Distributing Co., Lockport, NY, or The Lcncla Co., has been found suitable for this purpose. 5 Similar to U.S. Federal Specification Tr-P-650c Primer Coating Latex Base, White (for Gypsum Wallboard). 6.03 DUP050297784 # D 3928 * Direction of finishing brush strokes FIG. 1 Test Pane! or the following metric equation: g = [(Am x D)/SJ x 1000 where: Am = area, m2, D = density, g/mL or kg/L, arid = spreading rate, m2/Ij. Make the initial brush strokes in the direction of the length of the panel and finishing strokes acrdss :the width of the panel with the wet edge feathered. Corriplete the painting of this section in about 45 s. Nuv' --This test method can be modified for roller application by using a small 3-in. (75-mm) roller instead of the 2-in. (50-mm) brush to rank the uniformity ofaseries ofpaints when applied by roller. The 1-in. (25-mm) brush should still be used for touch up. 6.4 One minute after completing the painting of section A, apply paint to section B with the same brush still wet with the test paint. Use the same amount of paint and time to coat section B as .for section A but make initial brush strokes across the width of the panel and finishing strokes along the length of the panel. Brush the finishing strokes into section A overlapping this section by about 2 in. (50 mm) (see Fig. 1, area C). 6.5 Thirty seconds after completing the painting of sec tion B, use the still-wet brush but without additional test material to cross brush a figure X on this section as shown in Fig. 1, area D. Air dry for at least 18 h under standard conditions. 6.6 Using the 1-in. (25-mm) brush and the spreading rate as in 6.2, apply the test paint to an area of about 3 by 5 in. (75 by 125 mm) of section A (Fig. 1, area E). This is to simulate a wall section that has been touched up after the previous coat has dried. Allow the completed test panel to dry a minimum of 18 h under standard conditions. 6.7 View low gloss finishes at a 5 angle to the plane oftbe' panel (85 to the normal) looking toward a strong light source. View gloss or semigloss coatings at 30 to the par,;! (60to the normal). Rotate the panel 360in the same plane while viewing in order to determine the overall appearance of the panel as viewed from different sides. Rate the test panel for gloss or sheen uniformity between sections using the following scale: Rating Score Excellent Very good Good Fair Poor Very poor A rating of excellent means that there is no discernible variation in .gloss or sheen between different areas of the panel. A rating of very poor means that there is a great s| variation in gloss or sheen between different areas. ,6.7.1 Variations in gloss or sheen may be caused by' various paint and substrate properties and application tech niques so that lapped, cross-brushed, and touched up anus will not necessarily have the same degree of sheen or gloss uniformity and it may be advantageous to rate each of these11 areas separately. 7. Interpretation of Results 7.1 The uniformity in appearance of a wall can be estimated by evaluating the variation in gloss or sheen between areas A and C of the test panel. 7.2 The uniformity in appearance ofa paint that has been applied by brush in different directions can be estimated by evaluating the variation in gloss or sheen between areas B and D. 7.3 The uniformity in appearance oftouched-up areas can 604 DU P050297785 D 3928 . _ ,, ;stimated by evaluating the variation in gloss or sheen ilietween areas A and E, Precision .1 In an interlaboratory study of this test method in ih one operator in each of six laboratories tested three nts of different levels of uniformity of appearance, all six laboratories ranked the three paints in the same order of appearance but there were considerable differences between the actual ratings assigned by the laboratories to any one paint. The test method should, therefore, be used only for the comparative evaluation of a test paint against a mutually agreed upon control paint or for ranking a series of test paints. y*; A; '`Sr:f The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights asserted in connection with any Item mentioned In this standard. Users of thl3 standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either feapproved or withdrawn. Yodrcomments are Invited either forrevision ofthis standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committed, which you may attend. if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 191$ Race St., Philadelphia, PA 19103. it* o St Ig JSrSff ~ &1 I 605 DUP050297786 Designation: D 3960 - 91 Standard Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings1 This standard is issued under the fixed designation D 3960; the number immediately following the designation indicates the year of original adoption Dr, in. the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice provides measures of the volatile organic compound (VOC) content of solventbome and waterborne paints and related coatings as determined from the.quantity of material released from a sample under specified bake conditions. Nwx' 1--Other terms used as synonyms for volatile organic com pound are photochemically reactive organic compound (PROC) and volatile organic substance (VOS). 1.2 This practice provides a guide to the selection of appropriate ASTM test methods for the determination of VOC content. 1.3 Certain organic compounds that may be released under the specified bake conditions are not classified as VOC as they do not participate in atmospheric photochemical reactions. Such nonphotochemically reactive compounds are referred to as exempt solvents in this practice. 1.4 VOC content is calculated as a function of (7) the volume of coating less water and exempt solvents, and (2) the volume of coating solids. 2. Referenced Documents 2.1 ASTM Standards: D 1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products2 D2369 Test Method for Volatile Content of Coatings2 D2697 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings2 D2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings2 D 3792 Test Method for Water Content of Water Reduc ible Paints by Direct Injection into a Gas Chromatograph2 D4017 Test Method for Water in Paints and Paint Materials by Karl Fisher Method2 D4457 Test Method for Determination of Dichloromethane and 1,1,1-Trichloroethane in Paints and Coat ings by Direct Injection into a Gas Chromatograph2 D5201 -91 Practice for Calculating Formulation Phys ical Constants of Liquid Paints and Coatings2 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemicals3 2.2 Other Documents: EPA Federal Reference Method 24--Determination of Volatile Matter Content, Density, Volume Solids, and Weight Solids of Surface Coatings4 EPA 450/3-84-019, U.S. Environmental Protection Agency Procedures for Certifying Quantity of Organic Compound Emitted by Paint, Ink, and Other Coatings4 EPA 450/3-83-013R, U.S. Environmental Protection Agency Glossary for Air Pollution Control of Industrial Coatings Operations4 Addition of Four Halocarbons to List of Negligibly Reactive Organic Compounds5 3. Terminology 3.1 Definitions: 3.1.1 exempt solvent--organic compounds that do not participate in atmospheric photochemical reactions. 3.1.2 nonvolatile material--the solid material remaining after volatiles have been removed from a coating under, specified test conditions. 3.1.3 volatile organic compound (VOC)--any organij|!| compound that participates in atmospheric photochemical reactions. 3.1.3.1 Discussion--The definition of VOC adopt.J h the U.S. EPA and a list of exempt compounds are include^! in Appendix X3. '" 3.1.4 volatile organic compound content (VOC content)-^-! the mass of VOC released from a coating under specified test4 conditions. 3.1.4.1 Discussion--VOC content is expressed in this practice as a function of: (7) the coating volume less water and exempt solvents, and (2) the volume of coating solids: 4. Summary of Practice 4.1 The volatile content, density, water content, volume solids and exempt solvent content of the coating are deter- : mined in accordance with designated methods and instnic-;:; tions. For multicomponent coatings, the components are first mixed in the appropriate ratios and the applicable values;, determined on the mixture. These values are combined using/ 1 This practice is under the jurisdiction ofASTM Committee D-l on Paint and Related Coatings and is the direct responsibility of Subcommittee D01.21 on Chemical Analysis or Paints and Paint Materials. Current edition approved Oct. 15, 1991. Published December 1991. Originally published as D 3960 - 81. Last previous edition D 3960 - 90. 2 Annua! Book ofASTM Standards, Vol 06.01. * Annua! Book ofASTM Standards, Vol 15.05. 4 Available from the Superintendent of Documents, U.S. Government Printing Office, Washington, IX 20402. s Published in the Federal Register, January 16. 1989, Vol 54, No. 11, p. 1966 Available from the Superintendent of Documents, U.S. Government Printini Office, Washington, DC 20402. 606 DU PO50297787 D3960 ified equations to calculate the VOC content of the ' ASTM idustrial ition of ds, and Section Organic iatings4 itection Justrial Eligibly , lo not ainina un^cr rgariv, anital e<l b" ducted mt)-- idtesi ; i this water Eds. * >TE 2--In Reference Method 24, the U.S. EPA defines a Wiw'rhonie coating as any coating with rapre than 5 tc-water by weight W.Cvolatae fraction, and requires/allows water determination for fA'ictfsprne coatings only. rS.lpignificance and Use A! Bp This practice discusses applicable ASTM test methods Win the determination of the VOC content of paints and Kd coatings and provides equations for calculating the f content expressed as the mass'of VOC in: (I) pet unit j||B.h of coating less water and exempt solvents, and (2) jpiiit volume of coating solids. P? Volatile organic compound content is used to com- Ihc amount of VOC released from different coatings Jgjfffoi the same application; that is, to coat the same area fee same dry film thickness (assuming the same appliea- 'ypffidency). VOC content data are required by various regulatory cfcies`. PpP Only the expression of VOC content as a function of IR -volume of coating solids gives a linear measure of the ifeence in VOC released from different coatings used for gigme application. MjfrB 3--Thus assuming the same transfer efficiency, a coating with ('content of 3-lb of VOC/gal ofsolids would release V: the VOC that a Coating with 6 lb of VOC/gal of solids. >! K; When VOC content is expressed as a function of the Ipne of coating less water and exempt solvents/lhe-values ffined do not account for differences in the volume solids Jj|ht of the coatings being compared: this' expression. Spore, does not provide a linear measure ofthe differtfice 1VOC emitted, from different coatings used Tor the same ilication. " '' . y zS J<< ' 4--Thus, a coating with VOC content of 3 lb of VOC/gal less Iff and exempt solvents would release about 85 % less VOC than a ling with 6 lb of VOC/gal of solids; Nonvolatile and Volatile Content jp Guide D 2832 includes suggested time/temperatuie ring schedules for the determination of the nonvolatile ! volatile content of various types of coatings. $P{' 5--For regulatory compliance testing, follow the method and niitions specified in the applicable regulation. Federal Reference le'jibd 24 specifies the use of Test Method D 2369. .? Test Method D2369 includes a specific drying lipriule and sample weight, and heating. 1 h at 110 5C for "lelgrmination of the weight percent volatile;content of ijventborneawdwaterboxree.coatings. .. 6.2.1 For multicomponent coatings, Test Method D 2369 'Pacifies the components should be mixed fust, then ffie Virile content,should be determined bn the mixture. Test sptc'mens are held in the aluminum dish for at least 1 h before baking. |}N ' 6--U.S. EPA will allow the test specimens to stand at room temperature for up to 24 h prior to baking at 110 5C for 1 h. 7. Water Content 7.1 To determine the water content" of waterborne coat ings two test methods are available: 7.1.1 In Test Method D 3792, a paint specimen is diluted with dimethyl formamide, an internal standard (2-propanol) is added, and an aliquot of the mixture is injected directly into a gas chromatograph; 7.1.2 In Test Method D 4017, a paint specimen is diluted with pyridine and a catalyst (1-ethylpiperidine) is added to obtain a rapid and definitive titration end point. 7.1.3 With waterborne multicomponent coatings, the components are first mixed in the appropriate ratios, then water content is determined using Test Methods D 3792 or D4017. 8. Density 8.1 The density of the paint or coating at 25C is determined in accordance with Test Method D 1475. Al though, both the pycnometer and weight-per-gallon cup are covered by the test method, and the former is more accurate and precise, the weight-per-gallon cup is recommended because of its speed and ease of use. , 8.2 With multicomponent coatings, first mix the compo nents in appropriate ratios in sufficient quantity to deter mine the weight-per-gallon using Test Method D 1475. 9. Exempt Solvents "9.1 In Test Method D4457 ah internal standard (1propanoi) is added: to the tbst specimen, and then the specimen is injected directly into a gas chromatograph. 9.1.2 With multicomponent coatings, the exempt solvent content is determined on the mixture of the components. 10. Calculation of VOC Content 10.1 In this practice VOC content is expressed in two ways: {/) as the mass of VOC per unit volume of the coating less water and exempt solvents, and (2) as the mass of VOC per unit volume of coating solids. The following equations should be used to calculate VOC content and may be used for coatings both "as supplied" and "as applied" (see Note 7). ~N ' 7--For compliance with VOC regulations, the VOC content should he calculated after any thinning or dilution ("as applied"), instructions for VOC calculations of such diluted coatings are available in EPA 450/3-84-019. 10.2 VOC Content Expressed as the Mass of VOC per Unit Volume of Coating Less Water and Exempt Solvent: 10.2.1` General Expression: (weight percent of total volatiles less water less exempt solvents)(density of coating) VOC ----------- .---------- -----------1----------------------- ------------------------- 100 % - (volume percent of water) - (volume percent of exempt solvents) or 196b intin 607 DUP0502 97788 D 3960 (TO VOc = loo - E ,, - r (JVv - fVw - W,,)(flc) (1) 100 - (WJVDJD J - (i,,) where: VOc = VOC content in g/L of coating less water and exempt solvent (see Note 8), Wa = weight percent of organic volatiles, (Wv - - HU. f^v = weight percent of total volatiles, (100 % -- weight % nonvolatiles, see Test Method D 2369), Wv = weight percent of water, (see Test Methods D 3792 or D 4017), " = weight percent of exempt solvent, (see 3.1.3.!, Note 9, and Test Method D 4457), K, = volume percent of water, (Wf&DJD ,,), - volume percent ofexempt solvent, (see 3.1.3.1, Note 9), = (W'K){DJD ex), J>e = density of coating, g/L, at 25C, (see Test Method D 1475), A* = density of water, g/L, at 25C, (0.997 x 103), and A* = density of exempt solvent g/L, at 25C, (see Test Method D 1475). Nora 8--To convert from g/L to lb/gal, multiply the result (VOC content) by 8.345 x 10-3 (Ib/gal/g/L). To convert gfL to kg/L, divide the result by 103. N' 9--See Appendix X2.1 and X2.2 for comments on coatings containing one or more exempt solvents. 10.2.2 Solventborne Coatings--Calculate the VOC con tent in grams of VOC per litre of coating less water and exempt solvents using the appropriate equation: 10.2.2.1 For solventborne coatings that do not contain water or exempt solvents; voc (FVvXA,) 100 (2) 10,2.2.2 For solventborne coatings that contain an ex empt solvent but do not contain water (see 3.1.2.1 and Note 2): VOC = (H^v - WKOc) m-(W,,)[DJDn) 10.2.2.3 For solventborne coatings that contain water but do not contain exempt solvents (see 3.1.3.1 and Note 2): (IVv - WJ(DJ VOC* 100 - (WJ(DJDJ W 10.2.2.4 For solventborne coatings that contain both an exempt solvent and water, use pq 1 in 10.2.1 (see 3.1.3.1 and Note 2). 10.2.3 Waterborne Coatings--Calculate the VOC content in grams of VOC per litre of coating less water and exempt solvent using the appropriate equation. 10.2.3.1 For waterborne coatings that contain no exempt solvents, use Eq 4 in 10.2.2.3 (see 3.1.3.1 and Note 2). 10.2.3.2 For waterborne coatings that contain exempt solvents, use Eq 1 in 10.2.1 (see 3.1.3.1 and Note 2). 10.3 VOC Content Expressed in Terms of the Mass of VOC per Unit Volume of Coating Solids (Nonvolatiles): 10.3.1 Calculate the VOC content in grams of VOC per litre of coating solids according to the following equation: (Wa){Dc] VOCm = where: VOCm = VOC content in g/L of coating solids, *,f K = Wv - Ww- Wex (terms defined as in 10.1.1), and)| V,, = volume percent of nonvolatile content of the liquid coating, (see Test Method D2697, and Notes 10 and 11). N' 10--The EPA Reference .Method 24 does not include: an analytical method for determining F> but states that the value he calculated from the coating manufacturer's formulation. N' 11--An expression for calculating formula V,, from the coating formulation is included in Appendix X2.3, Eq X2.1. 11. Keywords 11.1 VOC; VOC calculations; VOC content; VOC con tent of paint; VOC content, test precision APPENDIX fajha (Nonmandatory Information) XI. AUTOMOTIVE COATINGS SUPPLIERS ROUND ROBIN XL I A round robin was conducted at the laboratories of automotive coatings suppliers for determination of VOC using Practice D 3960. The analysts involved were persons experienced in running all the test methods involved in,VOC determination. The data was analyzed statistically in accor dance with Practice E 180. As was suspected from previous round robins conducted to evaluate Practice D 3960 (which involved some laboratories not familiar with these test methods), when well experienced analysts conduct the tests, the precision data is much improved. X1.2 The interlaboratory study involved four laboratories and six samples; four solvent-reducible automotive topcoats and two water-reducible automotive topcoats. One operalo. in each of the four laboratories analyzed the sample in duplicate on 2 different days. The following duplicates, repeatability, and reproducibility coefficients of variation were obtained. Automotive Topcoats Duplicates, Repeatability, % Reproducibility (Within (Between Laboratory) Laboratory) Solvent-reducible 0.86 1.62 2,86 Water-reducible 3.94 5.29 9.75 608 DU P05 02 97789 # D 3960 X2. CALCULATION OF VOC CONTENT (SECTION 10) jjj 2.1 Measurement of Exempt Solvent Content--The 5 of the weight percent or volume percent of exempt jgnt in the VOC expression (Eqs l, 3, and 5) can be Untied using Test Methods D4457 and D 1475 if the ent is methylene chloride or 1,1,1-trichloroethane. 2.2 Two or More Exempt Solvents--For solvent or |l:-reducible coatings containing more than one exempt wnt, the values for Ex and (Ex){DJDCK) to be used in Eq ' <'0.2.1, 10.2.2.2, 10.2.2.4 or 10.2.3.2} are the ^S&inmations of the values of Ex and (Ex)(DJD^'d for each jlidual solvent. Also, the value for Ex to be used in 10.3.1 determine V0 in Eq 5) is the summation of the individual plues. .3 Volume Nonvolatile Content--The volume percent Volatile content, K,,, in Eq 5 (10.3.1) can be calculated the summation of the individual contributions of each .ponent in the coating formulation ("p" components) | the following equation (Notes X2.1 and X2.2): % = 2 [([ fnJiX Vyf 100)] (X2.1) % -- volume percent of nonvolatile component "j," [(100 %) x (volume of nonvolatiles of "j" per unit volume of "j")], and - volume percent of component "j'' in the coating [(100 %) x (volume of "j" used)/(total volume of coating)]. X2.1--Instructions for calculating the value for the formula at volume solids (or formula volume percent nonvolatile) content lb" c rating are provided in Practice D 5201. N' X2.2--Eq X2.1 is meant to clarify the equation (H-4) currently in the EPA certification manual EPA-45Q/3 84-019 for the expression of calculated volume percent nonvolatile content, X2.4 Amount of VOC in a Coaling Expressed in Terms of Mass of VOC per Unit Volume of Coating Including Water and Exempt Solvents--The amount of volatile organic compounds in both solvent- and waterborne coatings can be expressed in terms ofthe mass of volatile organic compounds per unit volume of coating including water and exempt solvents according to the following equation (Note X2.3) VOA = 100 (X2.2) where: VOA = Amount of volatile organic compounds in g/L of coating including water and exempt solvents. N' X2.3--Calculation of the amount of volatile organic com pound based on the total volume of coating (including water and exempt solvents), as illustrated in Eq X2.2, does not provide a measure ofthe amount ofVOC that would be released from two coatings used for the same application (that is, to coat the same area to the same dry film thickness assuming the same application efficiency for each coating) when one or both ofthe coatings contain water or exempt solvents. These units do not identify which of the coatings will release the greater amount of VOC as they treat water and exempt solvents as coating solids. These units, therefore, have not been used, recommended or accepted by U.S. EPA for demonstration of compliance with VOC content regulations as such calculations yield misleading results for coatings that contain water or exempt solvents. N' X2.4--The expression in X2.2 is useful for the calculation of the mass of VOC released per unit of time (for example, the mass of VOC per unit of volume including water and exempt solvents times the volume of total coating used per unit of time). This expression may also be usefhl for certain labeling purposes where the amount of VOC per unit container is desired. APPENDIX 3 X3. REGULATORY DEFINITION OF VOC 1X3.1 The regulatory definition of volatile organic coms (VOC) has evolved into the following statement by EPA.4-5'6 |X3.1.1 Volatile Organic Compounds (VOC)--Any or- c compound that participates in atmospheric photoical reactions; that is, any organic compound other n those which the administrator designates as having ligible photochemical reactivity. VOC may be measured a reference method, an equivalent method, an alternative thod, or by procedures specified under any subpart. A nee method, an equivalent method, or an alternative thod, however, may also measure nonreactive organic tanual on Determination ofVolatile Organic Compounds in Paint, Inks, and cti Products, ASTMManual Series, MNL 4, ASTM, May 39S9. compounds. In such cases, an owner or operator may exclude the nonreactive organic compounds when deter mining compliance with a standard. The administrator has designated the following organic compounds as negligibly reactive: methane, ethane, 1,1,1-trichloroethane (methyl chloroform), methylene chloride (dichloromethane), dichlorotrifluoroethane (HCF-123), tetrafluoroethane (HCFC-134a), dichlorofluoroetliane (HCFC-141b) and chlorodifluoroethane (HCFC-142b), trichlorofluoromethane (CFC-11), dichlorodifltioromethane (CFC-12), chlorodifluoromethane (CFC-22), trifluoromethane (CFC-23), tricblorotrifluoroethane (CFC-113), dichlorotetrafluoroethane (CFC-114), and chloropentafluoroethane (CFC-15), N' X3.1--The regulatory definition, under the control ofthe U.S. EPA, can and will change. A proposal to add compounds to this list is under consideration. To ensure currency, contact the local air pollution control agency. 609 r r DUP05029779Q # D 3960 The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ere entirely their own responsfo/Wy. This standardis subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or foradditional standards and shouid tie addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your Wews known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 610 DUP050297791 Designation: D 3964 - 80 (Reapproved 1989) Standard Practice for Selection of Coating Specimens for Appearance Measurements1 This standard is issued under the fixed designation D 3964; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflasl rcapproval. A superscript epsilon (<) indicates an editorial change since the last revision or rcapproval. INTRODUCTION In making appearance measurements, it is important that the specimens selected be representa tive of the material of interest. Once selected, the specimens must be carefully examined to determine if they are suitable for measurement, and if not, they must be cleaned or otherwise prepared. Careful attention to these factors & necessary if the measurements are to be valid. Scope |1, This practice provides a guide to selection of specifli.for appearance measurement as well as a discussion of ps to be considered in their preparation for measure|L Standardized selection and presentation procedures (assist in achieving agreement between evaluations carjjjnit in different laboratories as well as helping to achieve correlations between visual evaluations and instrufial measurements. IjJiTE 1 --This standard is not a practice for preparation oftest panels Ratings; see Test Methods D 823. Ife This standard may involve hazardous materials, operwhs, and equipment. This standard does not purport to l^ess all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish ropriate safety and health practices and determine the ilicability ofregulatory limitations prior to use. ijReferenced Documents Jj.1 ASTM Standards: g> 823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on s Test Panels2 |E 284 Definitions of Terms Relating to Appearance of Materials3 Terminology 13.1 Definitions: B. 1.1 For definitions of terms used in this practice, refer to llinitions E 284. !; Significance and Use |4.1 Many of the specimens that are regularly submitted to neasuremen: depart in some degree from the ideal require- >*4 1 This practice is under the jurisdiction ofASTM Committee D-t on Paint and Tjgeiated Coatings and is the direct responsibility of Subcommittee DO 1.26 on ijpptical Properties. Ilf nirrent edition approved Oct. 31, 1980. Published December 1980. Annual Book ofASTM Standards, Voi 06.01. Annual Book ofASTM Standards, Vo] 14.02. meats. For this reason instrumental readings are affected importantly by, the manner in which specimens are selected and presented for measurement. Reproducible measure ments are facilitated by standardization and control of test conditions. S. General Requirements 5.1 Specimen Size--The minimum size is dictated by the size of the specimen port of the instrument to be used for measurement. When an instrument provides a choice of specimen port sizes, use the largest port that can be com pletely covered by the specimen. A large measured area helps to minimize the effect of any small area nonuniformity and is therefore more likely to provide results that agree with the involuntary averaging that takes place when specimens are observed visually. A large specimen also permits the operator to make measurements,, on several areas of-the specimen when desired thereby providing further specimen averaging. 5.2 Opacity-*-An opaque specimen shall be selected whenever possible for gloss and color evaluation. When the specimen is translucent or transparent, the following points should be considered: 5.2.1 For Gloss Evaluation--The specimen shall be suffi ciently thick that a secondary reflection from the back or second surface of the specimen cannot enter the receptor optics of the glossmeter. When thin transparent specimens must be measured, adopt one of the following procedures: 5.2.1.1 Back the specimen with a light absorbing material of the same refractive index as the specimen, and in optical contact with it. 5.2.1.2 Use an agreed upon specimen thickness, including coating and. substrate and place a black backing behind the specimen. 5.2.2 For Color Evaluation--The choice of backing of even slightly translucent specimens will affect their measure ment. Use the most applicable of the backing techniques that follow. In each case it is essential that the backing material and color be reproducible, stable, and durable for reliable results. 5.2.2.1 Back the specimen with the same material with which it will be backed in its intended use. 611 DUP050297792 # D 3964 5.2.22 Back the specimen with identical or similar mate rial. 5.2.23 Back the specimen with a neutral material whose luminous reflectance is essentially the same as that of the specimen being evaluated. 5.2.2A Back the specimen with a black surface such as a painted panel or black glass. 5.2.2.5 Back the specimen with a white backing of known reflectance. 6. Physical Properties 6.1 The specimen shall be rigid and have a plane surface. Specimens of thin, flexible material that can bulge or sag when presented to an instrument require special holding equipment When the specimen is moderately flexible, a plane surface may be achieved by pressing the specimen against the instrument with a flat, rigid object. The pressing technique must be reproducible. A vacuum plate or specially designed clamping device has proven satisfactory in some applications. Note that specimens coated on thin plastic film or paper may trap air between the specimen and the holder (vacuum plate or clamping device) causing the specimen to billow (blister) resulting in erroneous readings, 6.2 Surface Texture--Some coatings have pronounced surface texture, making it desirable to rotate a specimen in its own plane. Those with marked directionality, usually due to the production process, will have different values when measured in different directions. Good practice dictates that measurements be made with the plane of measurement of the instrument both parallel to as well as perpendicular to the process direction. 7. Cleaning of Specimens 7.1 The specimen must be clean. There should be no dirt, dust, oil or foreign material on the surface that will affect the instrumental evaluation of the specimen. If the specimen appears to require cleaning, the procedure should be agreed upon and it should be carried out with care. Any cleaning of a low-gloss or fragile surface may scratch or polish the surface and thus change the appearance of the specimen and render it useless for measurement. A high-gloss specimen <n usually be washed with clear water and blotted with untreated lens tissue or paper towel. If the specimen is durable, a mild nonfluorescent, nonionic detergent that doss not leave a film can be used with a soft cloth or bristle brush. If the specimen is durable and has an oily or stubborn contamination that should be removed, reagent grace isopropyl alcohol may be used. Follow ail cleaning tech niques with a warm water rinse and drying by blotting, usun; untreated lint-free paper towel. ' N' 2--Ceramic or porcelain enameled instrument calibration standards require periodic cleaning and the above procedures caa generally be used safely. 8. Handling Specimens 8.1 Handle specimens by their edges. Do not allow objects to contact the front surface of the specimen. When placing the specimen on the instrument, avoid sliding it across it. specimen port. 9. Report 9.1 When the specimens submitted for appearance measurements depart from the ideal requirements, report the following: 9.1.1 Their condition (Section 6), 9.1.2 Method of cleaning (Section 7), 9.1.3 Method of backing (5.2.1, 5.2.2, and 6.1), and 9.1.4 Indicate direction of specimen submitted for mea surement or averaging of data, or both, when required by directionality (6.2). The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ace entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprovedor withdrawn. Your comments are invited either tor revision of this standardor for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 191$ Race St., Philadelphia, PA 19103. 612 DU P050297793 Designation: D 3980 - 88 Standard Practice for Interlaboratory Testing of Paint and Related Materials1 This standard is issued under the fixed designation D 3980; the number immediately following the designation indicates the year of original adoption on in the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. degree ofreplication and repetition. The experimental design tt'Wfc 11 1 his. practice covers the interlaboratory testing of should provide the basis for an efficient statistical analysis of ..^Spain' and related materials. The information presented is the results (see Part B, Planning). ' ^(intended to assist task groups in the effective planning of 3.3 replication--the execution of multiple chemical or -.Jrpimd-robin test programs. physical determinations on the same specimen or physical *"'* 1 " Ihe various parts appear in the following order: measurements on the same panel at the same time, as closely A Definitions Planning Sections 4 3 to n as passible. Two replicates are called duplicates, three are called triplicates, etc. The individual results are not suitable for estimating precision but are used only to ensure by -Statistical Analysis 12 to 16 comparison with similar measurements that there is not.a I'--Analysis Presentation 17 to 20 gross error among them (see 15.1.3.3). This practice,, in spite of its length, is not intended to 3.4 repetition--The execution of multiple physical mea Jr all aspects of statistical design and analysis. For surements on the same panel or chemical determinations at fple, the analysis of variance used in the practice as the different times, or physical measurements on different for estimating the precision,is abridged in comparison panels, areas of large structures, or specimens of a liquid JUt normally used for establishing the significance, of sample within a short time interval, to establish the precision irimental factors. The publications listed in the appendix uld be consulted for further information or explanations, convenience, comparable practices developed by other p|M technical committees are also shown, of a method. In most cases the measurements are the mean of replicates as defined in 3.3. 3.5 population--the totality of observations on or deter minations of a certain, property or component obtained by Referenced Documents the same procedure; theoretically, an infinite collection of measurements on a given item of interest but, practically, a ASTM Standards: large number of measurements of the item. Thus, when |968 Test Methods for Abrasion Resistance of Organic statistical procedures are used-to determine whether or not jiGoatings by Falling Abrasive2 1-3793 Test Method for Low-Temperature Coalescence of Latex Paint Films2 M80 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial i Chemicals3 two (or more) materials or test methods differ significantly with respect to some measurable property, in effect, the determination is whether these materials belong to the same or to different populations. 3.6 sample--a randomly selected subset of a population intended to be representative of it so as to enable obtaining | PART A--TERMINOLOGY an estimate of the property or composition of the entire population. The reliability of such an estimate can be Definitions hi The statistical terms used in this practice are defined, parly as possible, in every day language. For convenience, Iterms are listed in order of use in this practice. 3,2 experimental design--the complete plan for conUcting an investigation or an interlaboratory study of iiiiterials, processes, or test methods. It is conveniently set *"-th in the form of a single comprehensive table showing umber of laboratories, materials to be tested, test methods, umber of operators, testing conditions, time of testing, and expressed in terms of confidence limits (see 3.19). Through tests of significance (see 3.21), it is possible to state, with a specified degree of confidence, whether two or more samples are drawn from the same or from different populations. 3.7 average--a typical numerical value that attempts to summarize or reflect the location of a group of observations by a single number. While it is a measure of central tendency, it does not provide information on the variability of the individual observations. The following are different types ofaverages: arithmetic mean, weighted mean, algebraic mean, geometric mean, harmonic mean, median, and mode. 3.7.1 mean (arithmetic)--the value obtained by dividing f1 This practice is under the jurisdiction of ASTM Committee CM on Paint and plated Coatings and Materials and is the direct responsibility of Subcommittee the sum of a set of observations or results by their number. This value is an estimate of the mean of the parent 61,20 on Sampling, Statistics, etc. ,/ Current edition approved May 27, 1988. Published December 1988. Originally {gtblishcd as D 3980 - 81. Last previous edition D 3980-87. ^Annual Book ofASTM-Standards, Vof- 06.01. A Annual Book ofASTM.Standards, Vol 15.05. population. Although the arithmetic mean is affected by extreme values and therefore may not be typical, it is amenable to statistical treatment and is the most commonly used average. 613 DUP0502 97794 0 3980 3.7.2 median--the central observation in an ordered set that contains an odd number of observations or the mean of the two central observations in an ordered set with an even number of observations. The median is not distorted by extreme values so that where the observations are not symmetrically distributed it is a more representative average than the mean. 3.8 expected value--the mean of an infinite series of independent determinations on the same item obtained by the same procedure; also thought of as the true value that would be obtained if all extraneous variations were elimi nated. In practice, it can be closely approached by a finite series of tests, the number of tests needed being dependent on the extent of variation (scatter) of the observed values. 3.9 accepted reference value--a value that serves as an agreed-upon reference for measured values. It is derived as a theoretical value based on scientific principles or an assigned value based on experimental work by (a) competent national or international organization(s). N' --When the accepted reference value is the theoretical value, it is sometimes referred to as the "true" value. 3.10 accuracy--the degree of agreement of individual or mean measurements with the expected or accepted reference value. 3.11 error--the deviation of a measured value or group of measured values from the expected value or accepted refer ence value. 3.11.1 random error--the chance variation that occurs in all experimental measurements despite the closest possible control of all factors. It is characterized by the fortuitous occurrence of both positive and negative deviations from the mean or the expected value. The algebraic mean of the deviations'is zero in a large series of measurements. 3.11.2 bias--a systematic as opposed to, a random, error that contributes to the difference between the estimated mean of the population and the accepted reference or the true value. 3.12 dispersion--the variability (scatter) of the observed values, usually measured about some central value such as the mean. 3.13 range--the difference between the lowest and highest values in a set of observations or results. The range is a simple but useful indicator of the variability of test results. 3.14 outlier--an extreme value far enough from other results in a series to be suspected of not belonging to the particular population under consideration. Statistical criteria are available for judging whether a given outlier should be included in the analysis of results or discarded (see Section 13). Also called "wild," "rogue," "maverick." 3.15 variance--a measure of the dispersion of a series of results around their mean. The variance of the parent population is estimated by summing the squares of the individual deviations from the mean and dividing by one less than the number Of results. D< ( <o n--Since the variance of a set of results and the estimated'variance of the parent population are not equal because of different divisors (n for the set, n -- 1 for the population), the same symbol should not be used for both. 3.16 standard deviation--a measure of the dispersion of a series of results around their mean, defined as the positive square root of the variance. D< ( < n--The advantages of the standard deviation are that it is in the same units as the original results and is of the same order of magnitude as the deviations from the mean. The standard deviation is thg basis for most state ments of precision and may be obtained from an analysis of variance of results of an interlaboratory test program. 3.16.1 pooled value--the weighted mean obtained by combining in accordance with statistical rules two or more separate values shown to be members of the same (homoge neous) population. Variances, if shown to be homogeneous by appropriate statistical criteria, may be combined by weighting each variance in accordance with its degrees of freedom, summing them and dividing by the sum of the degrees of freedom. Standard deviations must not be arith metically averaged; they must be squared to convert them to variances, combined, and the square root taken to obtain the pooled value. 3.16.2 coefficient of variation--a measure of relative pre cision calculated as the ratio of the standard deviation to the . mean of a series of values, expressed in percent. 3.17 degrees offreedom--in a set or subset of observa tions, the number of values minus the number ofconstraints. In general, there is only one constraint--the number of; values. For example, a set of n observations can be arranged into g groups. The group degrees of freedom is then g - i because n'is already determined. Similarly the total df is n -- I (see Table 8). -3.18 probability--the chance of occurrence of an event expressed in terms of a relative frequency, a fraction, or a percent. For example,' the probability that a tossed coin will land head up is one in two, or 0.5, or 50 %. 3.19 confidence limits--the limits on either side of the1 mean value of a group of observations that will, in a stated fraction or percent of the cases, include the expected value. Thus the 95 % confidence limits are the values between which the population mean will be situated in 95 out of 100 cases. 3.20 confidence level--the probability level (usually with reference to a statistical table) with which the significance of differences between measurements is assessed. Thus, a differ ence that is significant at the 95 % level (0.05 probability level, sometimes called significance level) would represent a real difference 95 times in 100; however, 5 times in 100 a difference this large might arise by chance even with identical.)! material because of experimental error. 3.21 significant difference--a difference between two.) values, means, or variances that is shown by tests of. significance to be a real difference at the stated level of : confidence. 3.21.1 Student's l test---a statistical test for assessing the significance of a deviation from the mean or of the difference between two means. The /-value is based on the ratio of the observed deviation, or difference, to the standard deviation and is compared with tabulated /-values that indicate the frequency with which a difference of this magnitude should occur by chance in samples having the appropriate degrees of freedom. 3.21.2 variance ratio (V) test--a statistical test for as sessing the significance of the difference between two or more variances. The F test (named in honor of R. A. Fisher) is based on the ratio of the larger variance to the smaller 614 DU P0502 97795 D 3980 flatus ties of s beea: ries ofi three " quite-i}i ratory tso I* Man STOs itorv mhor :nals I ar tfj -thoi* nter *UQv gl^Laboratory Pfe- i 1 ||' 11 If.5 etc. to h> mid be - 4 % itjBT fe u Experimental Design for Evaluation of a Single Method Using One Type of Apparatus Operator A Repeat 2 Replicate a b a Materials 23 b a b B 2a b a b A 2a b 1a b B 2a b etc. to a b A 2 a b 1a b B 2a b M FIG. 1 Example of Design for Iriterlaboratoiy Study W-* Bp a ' s, lls fiiiaterial beforb dividing1 them into groups to be distribp;}among the laboratories. Where necessary, the same ciiriCns may be sent in ttirn to each participating labora- ijjjlgB 2--Test panels arte frequently prepared in one laboratory to fish the variability only of measurements obtained in different |atories. Consequently, if panel preparation has a significant effect st results, the resulting precision win be better than where panels Sependently prepared by each laboratoiy. If, because of difficulty tabling a sufficient quantity, the same test panels are circulated to icipants, the test method may, depending upon the variability of H|. preparation and the sensitivity of the test method, also appear precise than if different panels were sent to each participant Jpl.4.1 Effect of Aging--If the specimens are such that jplir properties may change noticeably in a few days or fetefcs, coordinate the tests among the laboratories so that .i laboratory performs the test on specimens of the same ggs. fl,5 Report Form--Supply each laboratory with report jjprms like Fig. 2 to ensure that all results and pertinent information are reported in a uniform manner. In addition to space for measurement results, the form should provide space for such information as: relative humidity, tempera ture, instrument type, deviations from the specified proce dure, unusual observations, and constructive comments, as required. PART C--STATISTICAL ANALYSIS OF INTERLABORATORY TEST RESULTS 12. Scope 12.1 Appropriate statistical methods are described for computing the correlation, precision, and sensitivity of a test procedure from interlaboratory test results. 12.1.1 Outliers--For each material, ranges are computed between replicates run at each time by all laboratories, between means for each time for each laboratory, and between laboratory means of all repeats (usually two or three). Results from the different materials exhibiting similar variability or having similar mean values can be grouped and the ranges for each material calculated. For each type of range, the results are examined for suspected outliers and the 617 DUP050297798 D 3980 Report Form lor Interlaboratory Tests ASTM Subcommittee j------ . Task Group -- Interlaboratory Test on____________________________ Material 2 etc. to M Test Method 1A Repeat 1 Operator Replicate a b etc. to r Mean A. B A B A B Date received - --Date tested - Method of application (If required) - Film thickness (if required)------------ Film thickness method (if required)________________ Test temperatureRelative humidity _ Equipment description: Name___________ . Model No. - Comments: a Repeat 2 Replicate b etc. to r Mean Name - . Laboratory _ * ff more than one test method being studied. 0 If more than one operator per laboratory or locale. FIG. 2 Report Form test described in 13.3 applied, as illustrated in 15.1.3.4 and 15.1.3.5, to determine whether any values can be rejected. 12.1.2 Correlation--If a test procedure is being evaluated for its ability to provide results that correlate with the known property values of materials, a correlation coefficient is computed and tested for significance. 12.1.3 Precision--The precision of a test procedure is determined by computing intralaboratory and interlabora tory variances from the test results obtained for each material. If the variances for the materials are homogeneous, they are pooled and an overall intralaboratory standard deviation and an overall interlaboratory standard deviation are calculated and used in the precision calculations. If the variances are inhomogeneous, means of providing homoge neity (such as use of the coefficient of variation or other transformations of the results) are given. 12.1.4 Sensitivity--A sensitivity criterion (figure of merit) is computed and used as a measure of the ability of a test procedure to distinguish between materials differing in the property being measured. 13. Test for Outliers 13.1 An outlying observation, or outlier, is one that appears to deviate markedly from other members of the set in which it occurs. This outlier may be a single valui', mean, or a range. 13.2 When the experimenter is clearly aware that a gi deviation from prescribed experimental procedure has taken place, the resultant observation should be discarded, whell a it agrees or not with the rest of the results. If a relia correction procedure is available the observation may c corrected and retained. 13.3 In many cases, evidence for deviation from the., prescribed procedure consists of the discordant value itsci' In such cases a statistical test is applied to determine if the**1: 3 doubtful value should be discarded. A simple technique for, [ this purpose is the rejection quotient procedure. It consists of U) ranking the values (single observations, means, or ranges),.1 in order of their magnitude; (2) taking the difference betw.een the extreme value and the nearest value to it, and (3) dividing that difference by the appropriate range of urn values. The resulting quotient, Q, is compared with the established rejection quotient (RQ) for the number of items in the series of values. If Q exceeds the RQ, the extreme value is suspect and may be discarded. Table 1 gives the equationKrfj for computing Q and the RQ values for three significances! levels as a function of the number of items in the test results. It is recommended that outliers be discarded on the basis off the 0.01 significance level for intralaboratory results and the" 618 DU P050297799 D 3980 TABLE 1 Table for Testing Extreme Values -If 0 exceeds the rejection quotient, the suspect value may. be of Spues Ratio Significance Level* 0.10 0.05 0.01 Jg3 w* |fy5: 5G '/ *s I|.9 m 2 ii gRifyfrU-.3 $pi. 117C Ifcl8 ptfig NgrEo Pr I 2212 iwPtf&y*2V254J Bps WC * 2276 4 2D HfSO oO II li & 1I >< or Xn " Xn--1 Xn ~ X-f X,, -X, T >< 1 x,,_, -x, or x,,-x2 n= X3-X, rtr ^ -- Xn-2 X,,-a - X, x,,-x3 0.941 0.765 0.642 0.560 0.507 0.970 0.829 0.710 0.628 0.569 0.994 0.926 0.821 0.740 0.680 0.544 0.608 0.717 0.503 0.564 0.672 0.470 0.530 0.635 0.445 0.502 0.605 0.423 0.479 0.579 000000......454555806631309983 000000......655555164281156964' 0000.,..666697427077 00..569140 0.457 000...444432656 0000..:.444311098026 0000....333377888393 0.501 00..447809 0000....44446554'193a 0.436 0000....444412127923 000...555568570 00..553454 00*.552176 000...554019205 00..448893 t or probability of rejecting a valid extreme result. m significance level for interlaboratory results. When twits from several materials with similar property levels are analyzed, all the results must be included in the pilation of Q. Also, the test should be applied only once to lof laboratory results. Although two or more values can |f|jected at the same time, the remaining results should again be tested for outliers. i.4 Following is an example of the use of the rejection p!ient procedure for evaluating extreme values: 13.4.1 In the evaluation of the precision of a test method, nplc was tested within a single, laboratory twice on each two days by each of two operators for a total of eight erminations. Differences between replicates for both opprs on both days are ranked as follows: i 2345678 0.7 3.4 3.9 4.6 5.2 6.0 6.7 7.0 jp of the differences between replicates (the smallest !(Terence) appears to be suspect. I tom Table 1, for eight items: ''<? -{X2 - *,)/(*,,_, - *,) " (X2 - X,)/(X7 - X,) = (3.4 - 0.7)/(6.7 - 0.7) = 2.7/6.0 = 0.450 To reject one of the eight differences, Q must exceed 0.544 at id 0.10 significance level (90 % confidence level), 0.608 at EHfe 0.05 significance level (95 % confidence level), and 0.717 liie 0.01 significance level (99 % confidence level). Since a significance level of 0.01 should be used for iiitralaboratory (lest results, it is concluded that the difference of 0.7 is not fejectable and must be included in the calculation of test .precision. 14. Correlation 14.1 To be useful, a test method must provide values for materials that either relate directly to the known property or component values for these materials or that relate to the values from another test method that is related to the known values. The degree of association between the values of a test method under study and the values ofa standard test method can be determined by computing the correlation coefficient. 14.1.1 The correlation coefficient, r, may be defined by the equation: 2(X-X)(Y- Y) ` [2(X.-X)22(Y- Tfp' 2XY-_ (2X2Y/n) where: X = value obtained for a material by standard test method, Y = corresponding value obtained for a material by new _ lest method, X -- mean value obtained for a material by standard test _ method, Y = mean value ^'obtained for a material by new test method, and n -- number of values obtained with each test method. 14.1.2 The reliability of the correlation coefficient de pends on the number of materials tested as well' as the degree of linear relation between the two test methods. It should be pointed out that a calculated r value represents the relation of the two test methods only over the range of values obtained. Thus, if the material? selected for evaluating a test method differ only slightly in their property or component levels, the calculated rmay not correspond to the correlation that would be obtained if materials differing widely in these values had been tested. 14.1.3 The correlation coefficient, r, is dimensionless and its values range from 1.0, perfect direct relation, to -1.0, which indicates perfect inverse relation. An r of 0 shows no relation between the two test methods. Whether a value of r between 0 and I is significantly different from 0 can be determined from Table 2 that gives the critical values at several probability levels as a function of the degrees of freedom, n -- 2, where n is the number of materials tested. 14.1.4 The correlation coefficient squared, r2, (called the coefficient of determination) provides additional informa tion about the degree of correlation between the two test methods. It is a useful concept in the sense that r2 is equal to the fraction of the variation ofthe dependent variable Y that may be ascribed to the effect of the independent variable X. To claim good correlation exists between two test methods, a value ofat least 0.9 for r is required, since r2 = 0.81 indicates only 81 % of the variation in Y can be ascribed to X. If a value of 0.7 or less is obtained for r, the degree of association is considered to he inadequate for assuming that the two procedures are measuring the same property. It should be pointed out that a high value for r does not guarantee that values of Y can be predicted precisely from vaiues of X. 14.1.5 An example of the computation of the correlation coefficient to determine the degree of association between values of two test procedures is shown in Table 3. Tills single laboratory test consisted of measuring the drying time of 10 619 4 :c -`- DUP050297800 D 3980 TABLE 2 Critical Values for Correlation Coefficient r Probability Level 4fA 0.10 0.05 0.01 1 0.988 0.997 1.00 2 0.900 0.950 0.990 3 0.805 0.878 0.959 4 0.729 0.811 0.917 5 0.669 0.754 0.874 6 0.621 0.707 0.834 7 0.562 0.666 0.798 8 0.549 0.632 0.765 9 0.521 0.602 0.735' 10 0.497 0.576 0.70B 11 0.476 0.553 0.663 12 0.457 0.532 0.661 13 0.441 0.514 0.641 14 0.426 0.497 0.623 15 0.412 0.482 0.605 16 0.400 0.468 0.590 17 0.389 0.455 0.575 18 0.378 0.444 0.561 19 0.369 0.433 0.549 20 0.360 0.423 0.537 A Of = the number of degrees of freedom (number of pairs minus 2). samples by two test procedures. The drying time values shown represent the mean of two replicate determinations. Since the computed r = 0.853 and r2 -- 0.728, it is concluded that the degree of association is adequate to assume that both procedures are measuring drying time because r exceeds TABLE 3 Example of Calculating Correlation Coefficient Sample 1 2 3 4 5 6 7 8 9 10 Sample 1 2 3 4 5 6 7 8 9 10 Total X 7 7.5 8 9 8 6 8 8 9 8.5 79.0 Drying Time, h Thumb and Forefinger Thumb and Balance 7 7.5 8 9 6 6 B 8 9 8.6 Y XY 7 7.5 7 9 8 6.5 8 9 9" 8.5 ' Xs , ya 7 49 49 49 7.5 56.25 56.25 56.25 7 56 64 49 9 81 81 81 8 64 64 64 6.5 39 36 42.25 8 64 64 64 9 72 64 81 9 81 81 81 6.5 72.25 7225 72.25 79.5 634.6 631.5 639.75 r /r ZXY-(2XX ZY/n) {ZXAr (S y)V/2 634.5 - [79 x 79.5/10) R631.5 - 624,1X639.75 - 632.025)]* 634.5 -- 628.05 6.45 [[7.4X7.725)]* 57.165* =Mr- as3 f3 = 0.728 0.765, the critical value at the 99 % confidence level for lo samples (8 degrees of freedom) in Table 2. 14.2 There may be instances where no actual instru mental values are available for the materials tested, only their relative ranking being known. In these cases, a rank correla tion coefficient, rj, can be computed to express the degree of relationship between the ranking of the X values of one test method and the Y values of the other test method. 14.2.1 In computing r/, the results from the two proce dures are each arranged in order of performance and each material assigned a rank. In the cases where two or more materials have the same rank, each is assigned the value corresponding to the mean of the ranks that would be assigned to them if the rankings were sequential. By taking the differences, RD, between the two sets of rankings for liie materials, rj is calculated from Spearman's equation a, follows: r; = 1 - imRDfhin'1 - 1)] = 1 - m(RD?Hn3 - )] where: n = number of materials and RD = difference between the rankings of a material. A test to determine if r/ is significantly different from 0 can be made conveniently with Table 4 in which S(RD)2 values at two probability levels are given as a function of the number of pairs. 14.2.2 An example ofthe procedure for computing a ra 1 correlation coefficient is shown in Table 5. In this example, the performance of 10 products subjected to two test procedures is represented by a relative ranking of thuperformance. It is seen from the significance table of S(RD)2 as a function of number of pairs that the value off 1 obtained: in this example is highly significant (99 %) since S(RD)2 u less than 39 for the probability level of 0.01. It is concluded that the degree of association between the two test procer' dures is good. 15. Precision 15.1 The precision of a test method is expressed in two terms, repeatability and reproducibility. Paragraphs 15.1.1 and 15.1.2 provide the complete mathematical formulas calculating precision, but a shortened procedure for analysis^ of results from a balanced design is given in 15.1.3. Whcit `, values have been discarded as a result of application'of tl-, test for outliers in 13.1, the mean of all the values for the-;;Ji respective determination can be used to replace them. retain a balanced design. It should be recognized that the analysis used in this practice is abridged because interactionsbetween factors are disregarded. Consequently, some infor mation that could be obtained from a complete analysis .s sacrificed, as in Practice E 180. 15.1.1 Repeatability (Intraboratory)--Test repeatability i' determined from the estimated intralaboratory variances computed from the repeat determinations made within each laboratory on each material. 15.1.1.1 For this practice, the equation defining the esti mated variance, xw2, (Note 3) within a single laboratory is as follows: = 2(Xt - - 1) 620 DUP050297801 # D 3980 * for 10 instn.. ily their correlaegreeof Me test proce ed each i r more : value uld be taking for the ion as TABLE 4 Critical Values of S(fiD)2 for the Rank Correlation Method Probability Level Probability Level 0.06 0.01 0.05 0.01 5 ,6 7 8 9 10 . 11 12 13 14 15 16 17 18 19 20 21 22 0-40 4-88 12-100 22-146 40-200 61-269 86-352 121-451 163-565 213-697 272-848 342-1 016 423-1 209 515-1 423 621-1 659 740-1 920 873-2 207 1 022-2 520 0-70 4-108 10-158 24-216 39-291 5B-3B2 84-498 115-613 154-756 201-919 257-1 103 322-1 310 398-1 540 484-1 796 583-2 077 695-2 385 820-2 722 23 24 25 26 27 26 29 30 31 32 33 34 35 36 37 38 . 39 40 1 187-2 861 1 370-3 230 1 570-3 360 1 789-4 061 2 028-4 524 2 287-5 021 2 569-5 551 2 873-6 117 3 199-6 721 3 550-7 362 3 926-8 042 4 328-8 762 4 757-9 523 5 213-10 327 5 698-11 174 6 213-12 065 6 768-13 002 7 334-13 986 960-3 088 1 115-3 485 1 287-3 913 1 475-4 375 1 681-4 871 1 906-5 402 2 149-5 971 2 414-6 576 2 700-7 220 3 008-7 904 3 338-8 630 3 693-9 397 4 073-10 207 4 476-11 064 4 908-11 964 5 366-12 912 5 853-13 907 6 367-14 953 of rabfe--If tiie observed total.SJRD)2, for the number of ranked pairs, n, is equal to or less than the lower tabular value, or equal to or greater than the higher r value, the correlation Is significant for the indicated probability. High values correspond to negative correlations, tow values to positive correlations. 0 can values of 11^1y' li a rank tmpi, 5 test thedr/l i :aine4' ' D>2i!4 'udeo roce- 1 2 3 4 5 6 7 8 9 10 Panel Designation Hjurel exposure rank ^clic.exposure rank iPIffeience (flD) difference squared (RD)2 TABLE 5 Example of Rank Correlation Calculation Ranking of Panels Subjected to Natural Exposure 8 C A D E and F H G I J Cyclic Condensation A and B D C E F^and H G J 1 A B CD E F GH 1 J Total 3 1 2 4 S.5 5.5 8 7 9 10 55 1.5 1.5 4 3 5 6.5 8 6.5 10 9 55 1.5 -0.5 -2 1 0.5 -1 0 0.5 -1 1 0 2.25 0.25 4 1 0.25 1 0 0.25 1 1 11 Rank total = (n(n + 1)/2) = (10(11 )/2) =* 55 * 1 - [62(RDf/in3 - n)] = 1 - R6 X 11)/<1000 - 10)3 = 1 - (66/990) =,1 - 0.067 = 0.933 material by the analysis of variance technique, described in = value obtained in a single determination for 15.1.3. If the results are not balanced, the computations are a material by: a laboratory, made on the repeat determinations performed within each == total number of repeat determinations made laboratory on each material. on that material by a laboratory, 15.1.1.3 If, by inspection, the intralaboratory variances of _ = mean value for the nR determinations, all laboratories for a material appear to be homogeneous U'llN tor- :is is - Xf - sum of squares (ss), and 1 = degrees of freedom, df. OFoase of computation, the equation is arranged as follows: (approximately the same) they can be pooled to give a single intralaboratory variance for that material. 15.1.1.4 If the intralaboratory variances for a material do not appear to be homogeneous, a statistical test, such as the Cochran4 or Bartlett5 tests, should be used to determine whether the variances can be pooled. irh (% - 1) IO' 3--The subscript, w, to the variance s2, as well as later to the 15.1.1.5 Pool the variances fbr all the materials (unless they appear to be nonhomogeneous) to give a single intra- lard deviation, s, and the coefficient of variation, r, derives from the csti- loOsly used term "within-laboratory". is as 5.1.1.2 When the results obtained in the interlaboratory 4 Cochran, W. G., and Cox, G. M., Experimental Designs, John Wiley and , . are from a balanced design and there are no missing Sons, New York, NY, 1957. 5 Youden, W. J., Statistical Methodsfor Chemists, John Wiley and Sons, New l^fues, compute the sums of squares and variances for each York, NY, 1951. 621 Il I DUP050297802 D 3980 laboratory variance for all materials. Obtain the intra laboratory standard deviation, tw, by taking the square root of the variance and report. 15.1.1.6 Compute the maximum allowable difference (MAD) by multiplying sw by the q factor (Table 6) for the appropriate number of replicates in each laboratory and the degrees of freedom (nm materials) x (nL laboratories) x (time -- 1). In case test results are missing, compute the nL (/ - 1) degrees of freedom for each material and total them. 15.1.1.7 Examine the results from each laboratory for each material to establish whether all results are within the MAD for intralaboratory determinations. If this range is exceeded and outliers were not previously rejected in accord ance with 13.3, discard the discordant results and recalculate the variance, standard deviation, and MAD. Compare with the original values to establish whether the rejection is justified; for example, a marked reduction in MAD with the elimination of only one set of results is evidence that they differ significantly from the other results and their retention would adversely affect the precision of the test method. 15.1.1.8 If the intralaboratory variances for the materials do not appear homogeneous but appear to be dependent on the level of the mean value of the materials, homogeneity may be achieved generally by converting the standard deviations to coefficients of variation: IV = 100 sJX 15.1.1.9 If the coefficients of variation are homogeneous, pool them in accordance with the equation, as follows: _ f(H| - 1) Vi2 + (m - 1) V22 + + (m - l)vro2lw Vp [ (,-l) + (2-l)+- -+(nm-l) J where: v, = coefficient of variation for Material 1, and i = number of values used to establish vb etc. When n, = n2 = nm, this condenses to (Svj2/m)% where: ZVj2 = sum of squared coefficients, and nm = total number of materials. Calculate the maximum allowable difference in percent relative by multiplying the coefficient of variation by q for the number of repeats and degrees of freedom. 15.1.1.10 If the coefficients of variation do not appear to be homogeneous, a transformation ofthe test results (such as to logarithms, arc sine, or square root) may provide homo geneous variances. 15.1.1. II If homogeneous variances or coefficients of variation cannot be obtained from the intralaboratory re sults, calculate the precision for appropriate levels of the materia] value. 15.1.2 Reproducibility (Interlaboratory)--Test reproduc ibility is determined from the estimated interlaboratory variance which is the variance of the mean values obtained by the laboratories (sL2) plus the intralaboratory variance. Thus, interlaboratory variance is as follows: i'b2 = (sw2/s) + where nK -- number of repeats in each laboratory. N' 4--The subscript, b, derives from the previously used tem, "between-laboratories". 15.1.2.1 The equation defining rw2 and the procedures for its computation are discussed in 15.1.1.1 and 15.1.1.2. 15.1.2.2 The equation defining the variance of laboratory means, sL2, is as follows: J>G2= nx-XfKn^- l) where: X X (X - X)2 nL - 1 = mean obtained for a material by a labora tory, -- grand mean of the values obtained for f material by all laboratories, = number of laboratories, = sum of squares, ss, and = degrees of freedom, df. To facilitate calculations, the equation is converted to , ZX2 - WWM L nL- 1 15.1.2.3 When the results obtained in the interlaboratory test are from a balanced design and there are no missingt values, compute the sum of squares and variance for each material by the analysis of variance technique, described in 15.1.3. Calculate the interlaboratory variance using the equation given in 15.1.2. 15.1.2.4 Pool the interlaboratory variances for all mate rials (unless they appear nonhomogeneous) to give a single interlaboratory variance for the test. Calculate the interiaboratoiy standard deviation, yb, and report. 15.1.2.5 Compute the maximum allowable difference try multiplying sb by the q factor (Table 6) for the appropriate number of laboratories and the degrees of freedom of (nL 1) times the number of materials. . 15.1.2.6 Examine the results from all laboratories toestablish that the range of laboratory means does not exci the MAD. If the range is exceeded and laboratory outlier- were not previously rejected, discard the discordant resultfej and recalculate the MAD as in 15.1.1.7. 15.1.2.7 If the interlaboratory variances for the mai 1 i do not appear to be homogeneous, but appear to vary with 'if the level of the means of the materials, convert the standard:^ deviations to coefficients of variation, and if homogene pool them as shown in 15.1.1.8 and 15.1.1.9. Calculate! MAD in percent by multiplying the coefficient of variation;; by q for the number of laboratories and degrees of free 15.1.2.8 If the coefficients of variation do not appc.ii . homogeneous, a transformation of the test results (such as toCj logarithms, arc sine, or square root) may provide hom<3ge;:>| neous variances, if neither variances nor coefficients o; ''l variation are homogeneous for the interlaboratory resultsrjl calculate the reproducibility for each level of test value of the materials as in 15.1.1.11 15.1.3 A nalysis of Variance ofBalanced Results: i 5. i .3.1 Where a design recommended in Part B has been used and balanced results are available (that is, no missing values from a balanced design or missing values replaced by.-, the appropriate mean value), the analysis of variance tech nique should be used to compute the intralaboratory (within) 622 DUP050297803 ? ! - ? W-s-S-S'M D 3980 term TABLE 6 Values of the Studentized Range (g values) for the 95 % Confidence Level sA nB 2 3 4 5 6 7 8 9 10 V 18.0 26.7 32.8 37.2 40.5 43.1 45.4 47.3 49.1 ?: 6.09 8.28 9.80 10.89 11.73 12.43 13.03 13.54w 13.99 C 4.50 5.68 6.83 7.51 6.04 8.47 8.85 9.18 9.46 4 3.93 5.00 5.76 6.31 6.73 7.06 7.35 7.60 7.83 r 3.61 4.54 5.18 5.64 5.99 6.28 6.52 6.74 6.93 c 3.46 4.34 4.90 5.31 5.63 5.89 6.12 6.32 6.49 ,7 3.34 4.16 4.68 5.06 5.35 5.59 5.80 5.99 6.15 3.26 4.04 4.53 4.89 5.17 5.40 5.60 5.77 5.92 3.20 3.95 4.42 4.76 5.02 5.24 5.43 5.60 5.74 t a 1-0 11 2. J 4. 3.15 3.88 4.33 4.66 4.91 5.12 5.30 5.46 5.60 3.11 3.62. 4.26 4.58 4.82 5.03 550 5.35 5.49 3.08 3.77 4.20 4.51 4.75 4.95 5.12 5.27 5.40 3.06 3.73 4.15 4.46 4.69 4.8B 5.05 5.19 5.32 3.03 3.70 4.11 4.41 4.64 4.83 4.99 5.13 5.25 3.01 3.67 4.06 4.37 4.59 4.78 4.94 5.08 5.20 re.. 3.00 3.65 4.05 4.34 4.56 4.74 4.90 5,03 5.15. 17 2.98 3.62 4.02 4.31 4.52 4.70 4.86 4.99 5.11 19 2.97 3.61 4.00 4.28 4.49 4.67 4.83 4.96 5.07 19 2.96 3.59 3;98 4.26 4.47 4.64 4.79 4.92 5.04 ),, 2.95 3.58 3.96 4.24 4.45 4.62 4.77 4.90 5.01 V 2.92 3.53 3.90 4.17 4.37 4.54 4.68 4.81 4.92 JO 2.89 3.48 3.84 4.11 4.30 4.46 4.60 4.72 4.83 2.86 3.44 3.79 4.04 4.23 4.39 4.52 4.63 4.74 2.83 ' 3.40 . 3.74 3.98 4.1B $ 2.80 3.36 3.69 3.92 ^ ' 4.10 2.77 3.32 - 3.63 3.86 : 4.03 jpf *= degrees of Jreedonr associated with standard deviation or coefficient of variation, r ? number of repeats for repeatability or number of laboratories forvepraduclbilty. 4.31 4.24 4.17 4.44 4.36 4.29 4.55 4.47 4.39 4.65 4.56 4.47 interlaboratory (between) variances.6 In the analysis, it tinst be ascertained that the intralaboratory variances and nnsvalues are consistent among the laboratories. Interlabjj|y values are not necessarily consistent, depending oiq the precision of the test method(s). Lack of consistency arise from a variety of causes, such as materials or jigpient. As noted in 3.3, the individual replicates are }Jjfcnly for determining gross errors in test results. *8J .3.2 Following is an example of the application of the ysis of variance to interlaboratory test results. In this |d robin, one laboratory coated, baked, and distributed Jlanels to five co-operators. Each co-operator received e panels and was asked to determine the Knoop hardness thfde different times within a given period to eliminate jnlti effects. The results submitted are given in Table 7. p5.ll .3.3 The, first step (whether using the analysis of Bounce or nqt) is to examine each replicate value for |ible errors. This is most easily done by calculating the e in results for each time and comparing the ranges at jlar levels in results. In the example given.here, in which , range appears to increase with increasing hardness, the gfits for each enamel must be compared separately, but in cs where the values for all materials are at about the same IM.1 all results must be considered together. The calculated Ages in the example are presented at the bottom ofTable 7. 15.1.3.4 Next, apply the test for outliers, 13.3, or the control chart technique (D3) of Practice E 180, to see if a suspect value can be rejected. When more than two replica tions are made at a time and only one result is divergent, that result can be discarded and the mean calculated from the remaining values, thus retaining the balanced design of the interlaboratory study. When only duplicate determinations are made it is usually necessary to reject both results. In the example, Replicate b of Laboratory V on Enamel A at Time 3 has caused the range to be larger than acceptable, possibly the result of inverting figures when taking the readings or preparing the report. The mean for Time 3 is therefore calculated from the two remaining values which changes the subtotal for Laboratory V to 3.9, the total and mean of Enamel A to 18.7 and 1.247, arid the Laboratory V total to 140.2. 15.1.3.5 The ranges between the mean results at different times and the laboratory means (or totals) are also examined for discordant results to see if any should be discarded before conducting the analysis ofvariance. In the example none are rejectable; although the mean (and total) for Enamel E obtained by Laboratory IV appears suspect, the calculated quotient does not exceed the R.Q. of 0.710 for a significance level of 0.05 and five values, as shown: 48.9 - 34.4 48.9 - 26.7 > 0.653 15.1.3.6 An analysis of variance is performed on the jp A Basic software program to analyze test results in accordance with this results obtained for each material by the test procedure, that g&fctice, even if values are missing or have been rejected as outliers, is available l&i ETM Information Services Inc., 1829 Chaine Court, Gloucester, Ontario, p|i2W6, Canada. Equivalent programs may be available from other sources. is, a total of six analyses. It is necessary to compute first the variances for each material because the variances may differ significantly for different types of materials or for different 623 DU P050297804 3980 laboratory variance for all materials. Obtain the intra laboratory standard deviation, jw, by taking the square root of the variance and report. 15.1.1.6 Compute the maximum allowable difference (MAD) by multiplying sw by the q factor (Table 6) for the appropriate number of replicates in each laboratory and the degrees of freedom (nm materials) x (nL laboratories) x (time -1). In case test results are missing, compute the nL (r - 1) degrees of freedom for each material and total them. 15.1.1.7 Examine the results from each laboratory for each material to establish whether all results are within the MAD for intralaboratory determinations. If this range is exceeded and outliers were not previously rejected in accord ance with 13.3, discard the discordant results and recalculate the variance, standard deviation, and MAD. Compare with the original values to establish whether the rejection is justified; for example, a marked reduction in MAD with the elimination of only one set of results is evidence that they differ significantly from the other results and their, retention would adversely affect the precision of the test method. 15.1.1.8 If the intralaboratory variances for the materials do nol appear homogeneous but appear to be dependent on the level of the mean value of the materials, homogeneity may be achieved generally by converting the standard deviations to coefficients of variation: vw = 100 sJX 15.1.1.9 If the coefficients of variation are homogeneous, pool them in accordance with the equation, as follows: = [(" ~ *) + ("2 ~ 1) V;2 + ' + frtm ~ Dv'm2]'^ P l (, - l) + (*2 - 1) + + (m - 1) J where: Vj = coefficient of variation for Material 1, and = number of values used to establish v,, etc. When rtl = n2 = nm, this condenses to (Xv2/nm)lA where: Xv2 = sum of squared coefficients, and nm - total number of materials. Calculate the maximum allowable difference in percent relative by multiplying the coefficient of variation by q for the number of repeats and degrees of freedom. 15.1.1.10 If the coefficients of variation do not appear to be homogeneous, a transformation ofthe test results (such as .Jo logarithms, arc sine, or square root) may provide homo geneous variances. 15.1.1.11 If homogeneous variances or coefficients of variation cannot be obtained from the intralaboratory re sults, calculate the precision for appropriate levels of the material value. 15.1.2 Reproducibility (Interlaboratory)--Test reproduc ibility is determined from the estimated interlaboratory variance which is the variance of the mean values obtained by the laboratories (sL2) plus the intralaboratory variance. Thus, interlaboratory variance is as follows: rb2 = (Jw2/) + where nR = number of repeats in each laboratory. N' 4--The subscript, b, derives from the previously used tennf "between-laboratories". ' 15.1.2.1 The equation defining s,,2 and the procedures fori its computation are discussed in 15.K1.1 and 15.1.1.2. 15.1.2.2 The equation defining the variance of laboratory 1 means, sL2, is as follows: 1 sL2 = Z(X-XfnnL 0 where: X X nL (X -- X)2 nL -- 1 = mean obtained for a material by a labora- J tory, -- grand mean of the values obtained for a | material by all laboratories, = number of laboratories, = sum of squares, ss, and = degrees of freedom, df. To facilitate calculations, the equation is converted to ,, 9 S-?2 ~ WXfM 15.1.2.3 When the results obtained in the interlaboratoiy test are from a balanced design and there are no missing i values, compute the sum of squares and variance for each material by the analysis of variance technique, described jn! 15.1.3. Calculate the interlaboratory variance using the * equation given in 15.1.2. 15.1.2.4 Pool the interlaboratory variances for all mater', rials (unless they appear nonhomogeneous) to give a single J interlaboratory variance for the test. Calculate the interlabo- ratory standard deviation, sb, and report. 15.1.2.5 Compute the maximum allowable difference by multiplying rb by the q factor (Table 6) for the appropriate 1 number of laboratories and the degrees of freedom of (L - i 1) times the number of materials. 15.1.2.6 Examine the results from all laboratories to.J establish that the range of laboratory means does not exc^e j the MAD. If the range is exceeded and laboratory outliers^ were not previously rejected, discard the discordant resullsi and recalculate the MAD as in 15.1.1.7. 15.1.2.7 If the interlaboratory variances for the materials | do not appear to be homogeneous, but appear to vary with# the level of the means of the materials, convert the standard,! deviations to coefficients of variation, and if homogeneous.*! pool them as shown in 15.1.1.8 and 15.1.1.9. Calculate the| MAD in percent by multiplying the coefficient of varial o by q for the number of laboratories and degrees of freedom," 15.1.2.8 If the coefficients of variation do not appea`f'1 homogeneous, a transformation of the test results (such as to f logarithms, arc sine, or square root) may provide homogeCa neous variances. If neither variances nor coefficients ofij variation are homogeneous for the interlaboratory resulK calculate the reproducibility for each level of test value of the,, materials as in 15.1,1,11 15.1.3 Analysis of Variance ofBalanced Results: 15.1.3.1 Where adesign recommended in Part B has been used and balanced results are available (that is, uo missmg values from a balanced design or missing values replaced by the appropriate mean value), the analysis of variance tech-:; nique should be used to compute the intralaboratory (within) 622 DUP0502 97805 Laboratory Enamel Repli cate Aa b c Mean Ba b c Mean Ca b c Mean Da b c Mean Ea b c Mean Fa b c Mean Laboratory Total Grand Total Enamel A S C D E F TABLE 7 Knoop Hardness of Baked Enamels (a) Summary of Test Results ! ------------- ii------------- 111 IV Time Time Time Sub Time' Tame Time Sub Time Time Time Sub Time Time Time Sub 2 3 total 1 2 3 total 1 2 3 total 2 3 total V !! Time Time Time Sub 2 3 total Materia! Total Mean tiv !vV 1.0 1.4 1.2 1.2 1.2 1.1 1.1 1.0 1.3 0.91 1.1 1.1 ! 1.1 1.0 j 1.1 1.0 12 1.0 1.4 12 1.1 1.2 1.4 12 1.0 1.3 1.3 1.3 1.3 1.6 1.6 1.5 1.4 1.3 1.7 1.6 1.3 12 1.3 1.3 1.5 2.1 1.6 1.2 1.1 ------- " \ , V, - 1.1 1.2 1.2 3.5 1.0; 1.1 1.1 32 1.2 1.3 1.2 3.7 1.4 1.5 1.5 4.4 1.4 1.3 1.5 4.2 19.0 1.267 4 2.5 2.6 2.6 2.7 2.3 2.4 2.6 2.3 2.8 2.8 32 3.2 3.0 2.9 3.0 2.9 2.9 3.1 2.9 2.6 2.6 2.6 2.5 2.6 2.9 2.4 2.6 3.4 3.0 3.1 3.3 3.2 2.8 32 3.4 2.8 3.1 32 3.4 2.9 3.6 3.1 3.3 3.4 3.4 2.6 2.4 2.6 7.6 2.9 3.0 3.1 9.0 2.8 2.5 2.6 7.9 3.3 32 2.9 9.4 3.1 3.4 1 3.3 9.8 43.7 4.7 4.8 4.9 4.3 5.0 4.6 4.5 4.9 4.6 4.7 5.7 52 4.9 5.3 5.7 5.1 5.5 5.3 4.5 4.6 4.0 4.0 4.4 4.3 4.1 4.5 4.3 5.7 6.2 5.6 6.0 6.0 5.7 5.7 6.4 6.1 4.7 4.6 ; 5.7 4.9 5.1 j 5.1 5.1 5.0 5.4 2.913 | 4.5 4.9 4.7 14.1 4.9 5.5 5.4 15.8 4.2 4.5 42 12.9 5.B 6.2 5.8 17.8 4.9 4.9 5.4 15.2 75.8 ~UT . 6.2 6.5 6.5 5.6 6.8 6.1 5.9 6.5 6.0 8.0 6.9 7.9 7.9 7.3 72 7.5 7.1 7.4 6.7 6.3 6.2 7.3 6.5 6.7 7.0 6.7 6.3 8.5 8.7 8.7 8.3 62 9.3 8.1 8.3 9.0 8.0 7.7 7.7 8.4 7.1 7.8 8.2 7.4 62 5.9 6.6 6.2 18.7 7.8 | 7.1 7.5 22.4 7.0 6.5 6.4 19.9 8.3 8.4 9.0 25.7 8.2 7.4 7.9. 23.5 110.2 8.6 8.6 9.5 8.2 9.2 9.2 8.1 8.9 9.8 11.09.4 102 10.4i 92 9.9 10.7 j 9.6 10.4 10.1 9.3 8.9 9.7 9.5 92 10.5 10.0 8.6 16.6 16.5 15.9 16.0 17.0 15.4 16.3 16.9 18.1 11.9 11.7 112 11.8 11.5 11.0 12.3 11.0 10.7 7.347 8.3 6.9 9.5 28.7 10.7 j 9.4 102 30.3 10.1 9.6 8.9 26.6 16.3 16.8 15.8 48.9 12.0 11.4 11.0 34.4 168.9 11.260 ^ 14.6 16.1 14.8 14.3 16.2 15.5 14.9 15.7 15.3 18.6 18.7 17.7 18.0 19.3 172 17.7 19.0 17.0 15.4 13.8 13.9 15.2 132 14.6 14.7 13.5 14.1 17.4 16.1 17.3 182 16.2 16.7 17.8 16.6 17.0 18.6 20.2 19.1 18.0 19.6 18.7 18.3 19.9 19.5 14.6 16.0 15.2 45.6 18.1 I 19.0 17.3 54.4 15.1 13.5 14.2 42.8 17.8 16.3 17.0 51.1 18.3 19.9 19.1 57.3 251.4 16.7|ll 116.4 135.1 115.8 157.3 144.4 j J | 669.0 : (b) Range of Triplicates at Same Time Number at Stated Level 0 C.1 0.2. 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 10 6 42 1 ... ... ... ... 1 1 0 5 5 4 ... ... ___ ... ... 2 36 4. 1 ... ... ... ,.*f ... ... ... 1 4 54 1 ... ... .. if? ... ... ... ... 1 4 6 3 1 ..... ... ... ... ... ... 2 64 2 1 For 15 values O = ^--^2. The only divergent range Is with Enamel A where <= 0.75. R.Q. at 0.01 significance - 0.647. levels of the property measured. The analysis of variance of test results is facilitated by the construction of an analysis of variance table as shown in Table 8. 15.1.3.7 After calculating the means for the replicates, rejecting outliers where necessary, prepare a table of the means, which are considered to be the individual results, for each materia] as shown in Table 9 for Enamel A. 15.1.3.8 Perform the computations outlined in Table 8 to obtain the total sum of squares and the laboratories and the intralaboratory sums of squares. For each material from the sums of squares and the degrees of freedom, compute mean squares and variances for intralaboratory and for laboratory means as outlined in Table 8 and shown by the example in pabie 9 N' 5--In this example, triplicate measurements were made so that R equals 3 but in cases where duplicates are sufficient (see 11.2.1) the laboratory total sums of squares and the laboratory mean variances are obtained using two as the divisor. The number of replicates does not affect nR. 15.1.3.9 Calculate the intralaboratory and interlabi standard deviations for each material as in Ta Determine the maximum allowable differences for each'aijM compare with the ranges in the results as shown in Table1'. If'! required, discard discordant results and recalculate, 15.1.3.10 If the standard deviations for the i materials are homogeneous, pool the variances and cv.lcuV: ' ttle overali repeatability and reproducibility, as described n 15.1.1.6, 15.1.1.7, 15.1.2.5, and 15.1.2.6. `j 15.1.3.11 If the results are not homogeneous, convert tbsjj standard deviations to coefficients of variation, pool and calculate the repeatability, as described in 15.1.1.%, ' fi?d 5` `2'7 shown m ^nnex Al- . . ... 15.1.3.12 Prepare a table showing the standard deviations;- coefficients of variation (if required) and the precision ;|j given in Table 11. -:1 (. sensitivity ,ii ,. i`| 16.1 If a reasonably linear relationship (r > 0.7) has been'1 624 j DUP050297806 D 3980 H3urce of Variance patories laboratory TABLE 8 Analysis of Variance Table Sum of Squares (ss) Degrees of Freedom (DF) Eq 1 - SXZ - (SX)z/n 71-1 Eq 2 = Zi.*r/n,, - (ZXf/n Eq 1 - Eq 2 *L-1 (n - 1) - (nu - 1) = n - nL Mean Square Expected Mean Square"1 SS/DF ss/DF 3W2 + 7!r Sl2 .267 !.913 0S3. .347 .260 total number of determinations, number of laboratories, inis number of determinations (repeats) by each laboratory, :;ium of individual results (usually mean of duplicates), ;um of squared individual results, sum of individual results, squared, = sum of laboratory totals, - intralaboratory varianoe, - variance of laboratory means, and v* (swe/nB) + sL2 * Interlaboratory variance. ^Occasionally, in an exchange where the intralaboratory variability Is very high without a corresponding large difference between laboratory means, subtracting sw2 + Or Su2 yields a negative result. Since a variance cannot be negative, the usual practice In such cases is to consider sL2 to be zero.7 Laboratory Time 1 Time 2 . Time 3 Laboratory Total n --15 nR = 3 Source of Variation llla/and total jratoriea !* * lli^ralaboratory >:Laboratorymeans .. . stion factor (2X)a/n TABLE 9 Example of ANOVA for Enamel A--Means of Triplicates* 1.1 1.2 1.2 1.7 1.63 Total ss 23.63 23.58333 23.31267 1,0 1.1 1.1 3T= 1.2467 Netss 0.31733 0.27067 0.Q46& 1.3 1.4 1.4 1.2 1.5 1.3 1.2 1.5 1.2 4.4 [XXf = 349.69 (2X)z/n = 23.3127 df Mean Square 14 4 0.06767 10 0.00467 0.06300 3 Time Total 6.2 6.3 6.2 XlR = 70.76 XLT2/n,, = 23.6833 Variance 0.00467 = sw2 0.021 = suz cory: 0.00467 == 0.08B3 Table 8, q for 10 df is 3.6S for three determinations. Therefore, the maximum acceptable difference (MAD) * 0.0683 x 3.88 * ((nations (each the mean of triplicates). Atl laboratories comply since the maximum range Is 0.2 for Laboratory V. 'atory: 0.265 0.27 for three /nR ^+ sL22 = 0- .00467- + 0.021 0.00155 + 0.021 = 0.02255 4f|=(0.02255)*- = 0.150 v.b4tae"** Vji^From Table 8, q for 4 df en laboratory means * 1.467 - 1.087 * 0.4 for Laboratories II and IV. ',, = 0.95 for five laboratorias. All laboratories comply since the maximum range t for Laboratory V, Time 3. ft ;d between instrumental values and known property or sA = estimated experimental error for a single instru ponent values for the materials tested by a test method, mental measurement, and certainty with which the test method can detect differ- sP pes in the parameter should be ascertained. - estimated experimental error for a known pa rameter value. , 16.2 A useful measure of this certainty is the sensitivity ^Jsnterion.8 This criterion, SC, is defined as In many instances sP is not available sothat sp and AP are assumed to be 1,0, which removes them from the equation. Blf" AA/AP Thus the ` tern 1.?. Kpherere: AP II>ns, liwfoek.:; t a-) s a /s p change in instrumental value A for a unit differ ence in known parameter P, -- J. and Wasserman, W., Applied Linear Statistical Models, Irwin, SC=AA/s a 16.3 The value used for sA depends on the manner in which the test is conducted. For example, if materials are tested by the same operator with a single instrument, sw is used. Where the materials are tested in different laboratories, sb is used. 16.4 In the case where it is desired to know which of two ||l|Qmewood> IL, 1974, p. 534. alternative test methods, A or B, has the greatest sensitivity k ts Mandel, J., and Stiefileir, R. D., "Sensitivity--A Criterion for the Comparison Methods of Test," Journal ofResearch, National Bureau ofStandards, RP2527, for measuring P, a sensitivity ratio, SR, is calculated as 1 531153, No. 3, 1954, p. 155. follows:8 625 DUP050297807 D 3980 TABLE 10 Summary for All Enamels A Enamel A B C D E F 2X 18.7 43.7 75.8 110.2 1B8.9 251.4 Total-- 668.7 sx2 23.63 128.75 388.20 621.38 2011.15 4267.24 (2X)`/n 23.3127 127.3127 383.0427 809.6027 1901.814 4213.464 Intralaboratory Net Total ss 0.3173 1.4373 5.1573 11.7773 109.336 53.776 Enanel ss df Mean Square = sw2 sw A 0.0467 10 0.00467 0.068 B 0.2267 10 0.0227 0.1605 C 0.620 10 0.062 0.249 D 1.3133 10 0.1313 0.3625 E 3.3133 10 0.3315 0.5755 F 6.1267 10 0.6127 0.763 Total--60 Interlaboratory Enamel A B C D E F df 4 4 4 4 4 4 Total--24 Mean Square 0.0677 0.3027 1.1343 2.616 26.6057 11:9123 nRsL2 0.063 0.280 1.072 2.485 26.174 11.30 Su 0.021 0.0933 0.3574 0.8282 8.7246 3.7667 2/"n 0.0016 0.0076 0.0207 0.0438 0.1104 0.2042 A See Annex A1 for discussion of statistical analysis. sf-Vnf? 23.5833 128.5233 387.58 820.0667 2007.8367 4261.1133 Net Laboratory sT^ 0.2707 ' ** 1.2107 4.5373 10.464 106.0227 47.6493 ' Mean 1.247 2.913 5.053 7.347 11.26 16.76 0.0226 0.1009 0.3781 0.872 8.8352 3.971 0.15 0.32 0.615 0.93 2.97 1.99 vwr% 5.48 5.17 4.93 4.93 5.11 4.67 vbl% 12.D5 10.90 12.11 12.7' 26.4 11.89 H mnl* .n W-Mi TABLE 11 Material 1 2 etc. to M Summary of Interlaboratory Test by Method. Indicating Intra- and Interlaboratory Agreement Standard Deviation Coefficient of Variation Mean Intralaboratory Interlaboratory Intralaboratory interlaboratory sw df df V,, vb . sc,A SC,,, AAj&P . Sa /Sp _ AB/AP Afl/ja Sp/Sp where, if SR is greater than 1.0, Test Method A is superior to B, and if SR is less than 1.0, Test Method B is superior. 16.5 Obviously, a sensitivity ratio should not be used to compare test methods unless it has been established that one of these test methods provides instrumental values that correlate well with known property or component values of materials. For example, if Test Method A has been found to give instrumental values (observed or transformed) that correlate reasonably well (r > 0.7) with known property values, then a plot can be made of Test Method B values versus Test Method A values for the materials tested. 16.5.1 If the plot of points shows a curvilinear relation ship, then the values for Test Method B should be trans formed to provide a linear relationship. When this has been done, the slope of the straight line relating the points is AA/AB and SR - slope/(sA/ss) 16.5.2 In some instances, the SR for two test methods will not be constant over the range of materials tested because of changes in the test errors with a change in parameter level. In such cases, an SR should be calculated for each '61 ih, parameter value levels. A plot of SR values versus paramefef > values is useful in comparing the sensitivities of the two test methods. PART D--ANALYSIS PRESENTATION 17. Scope 17.1 This part describes the essential requirements for ttal preparation of a comprehensive report on an ASTM cvopei-; ative test program, for. the guidance of working groups aotrjfi committees or for publication, and of the precision i f ment to be used in test methods. j 18. General Report Requirements 18.1 The essential requirements for a report on a cbop. ative test program are as follows: 18.1.1 The presentation in one document of details pe laining to the program, including a complete description off the experiment with a dear statement of purpose, tf" cedure, instructions, and list of participants. 18.1.2 The presentation of all the original results reporl by the participants, together with their comments. 626 DUP0502 97808 D 3980 jr It Laboratory : 1 II etc.to Sb L Column totals C Column means Material 1 Number of Determlna- tions Mean Range Material 2 Number of Determina- tions Mean by Method. etc. to Material M Range Number of Determina- K tions Mean Range - igSjjM p. 1.3 An integrated compilation of the results into tables IpSlrid iri the form of graphs or charts that may be studied to .'-'tfghtain a dear view of the experiment as a whole. -ijK 'tlS.1.4 The presentation, in the most concise form, of the '"red:.elusions drawn from an analysis of the results. #11*1 ft. l .5 The presentation of a summary, conclusions, or a * of recommendations. '.`11.2 The report should provide maximum ease of refer- jj|to the details of the experiment, of observing results in ggliposition, and the essential conclusions. The report hid be available to all members of the task group well in IjriCe'of meetings so that there is sufficient time for study Sdevelopment of new ideas for discussion at meetings. .1 la &j . >tats DP-* petM< pr j rte |Procedures for Preparing Summaries 3.1 For each material or each test method, prepare, a IpThat compiles in an orderly block arrangement the fits from all of the laboratories (including operators and B). A format based on the one given in Fig. 1, but modi- J|tb include means and ranges, can be used. Using the fen shown in Table 12, prepare,a table for each test ||||<l.giving the'laboratory mean values.and ranges for the ggleht materials. Prepare a table, for each test method jjg for each material the means, the intra- and interlabo- By standard deviations, the degrees of freedom, and, if fpcable, the coefficients of variation. The format can be I on parts of Table 10 or on Table 11. It should be gfht from this tabulation whether the standard deviation fi'with the magnitude' of this property; being measured ^consequently, whether the coefficient of variation is Iked. : ||2 An appropriate block of results may be compiled Jti frequency distribution table that can be prepared in fail different Ways as follows: 1.2.1; Tabulate the values in increasing order of magm- pnd express the frequency with which each value occurs . fraction or percent calculated by dividing the number of |s the value occurs by the total number of values in a ip, When a large number of values is being treated, they |be divided into classes of equal, range (for example, ten ||es) and the frequency of each class calculated. |9.2.2 Calculate the deviation of each value from the an value of its group noting the sign and tabulate these in Sir of magnitude. Calculate the frequency of each deviai|ks a fraction or percent of ail the values treated. When a ge number of values is being treated, the deviations may Iglvided into classes of equal range. jf.2.3 Frequency distributions may be expressed in a Emulative way by arranging the values in order of magni tude and summing at each stage ofthis arrangement the total occurrence of all values up to and including the selected stage. 19.2.4 Graphical presentations are very useful and concise allowing rapid inspection and judgment of a collection of related results. They may be prepared from all the results from an experiment or an appropriate segment to obtain a view of the nature of the distribution. Ifit is revealed that an adequate normal distribution exists, relatively simple math ematical treatments may be applied. Frequency distributions may be presented in graphical forin, as histograms whereby values or classes covering a range of values are plotted against their frequency, or as cumulative frequency graphs prepared by plotting at each point the cumulative frequency of all the values up to that point against the value at that point. One of the best ways of displaying results is the dot diagram.9 Figure 3 shows the relation ofdry-to-touch time to the day on which a test was made and to the type of drier used, and also shows the overall distribution ofthe results. It can readily be seen that there is definitely a difference between days but none between drier types, as compared to the overall distribution. 19.3 The final summary should be a description of results from the cooperative program, expressedsin terms of repeat ability and reproducibility stated with supporting informal tipn, that is, degrees of freedom. 19.4 Prepare a draft report, with the test results and their analysis, for deposit in ASTM Headquarters files. 20. Applicability and Precision Statements for Test ' Methods 20.1 T[he major functions of the interlaboratory test of a measurement procedure are the determination of: 20.1.1 The applicability of the procedure for measuring a property of a material or groups of materials, and 20.1.2 The precision with which repeated measurements according to the test method can be expected to be made. 20.2 Applicability implies bpth the correlation of a mea surable property with an unmeasurable property of a mate rial and the sensitivity with which differing levels of that property are discriminated by the test method. Correlation may be evaluated by means of a rank order correlation coefficient. Sensitivity may be evaluated by means of the sensitivity criterion (ratio of the range in property levels of a material to the standard deviation). As applicability, or 9 Box, G., Hunter, W., and Hunter, S., Statisticsfor Experimenters, John Wiley and Sons, New York, NY, 1978, p. 221. 627 DUP050297809 # D 3980 30 v> 75 = 70 i ^u 65 I 60 0 1 S5 o 50 45 234 Day of Test BCD Type of Drier FIG. 3 Illustration of Dot Diagram Overall Distribution M i' validity, of a test method depends on the magnitude of the values of correlation and sensitivity, as well as on the number of materials used in the interlaboratory test, inclu sion of a statement of applicability is recommended as follows: Applicability of Test Method--Based on measurements of materials having known qualitative ratings that range from____ to ---- (good to poor, for example) the rank correlation coefficient for the test method was found to be-----------and the sensitivity criterion was found to be 20.3 Precision is useful only if the applicability function of the test method is found to be favorable. Precision is defined as the degree of agreement among repeated indepen dent measurements of the same property. Statements of precision may be given in terms of the standard deviation, but this form is not very useful. In addition, when values obtained vary directly with the property levels of the materials tested, the coefficient of variation must be used to express the general precision. Statements of precision can also be expressed in terms of the range in values within which the correct value can be expected to lie a specified percent ofthe time. The most common precision index is the range that should not be exceeded for a stated number of results at a given confidence level, assuming that the frequency distribution is normal and that a random sample was used in the interlaboratory test. Because only a sample of the total population of measurements is obtained in a test, statements of precision should indicate the number of degrees of freedom and the number of observations that were used in the interlaboratory test to obtain the indicated values. 20.3.1 As can be seen from Tables 11 and 12, the measurements made in an interlaboratory test permit a number of parameter variations. Precision indexes can be devised with respect to differences within and among labora tories, materials, operators, and repeat measurements and with respect to the interactions among combinations of the parameters. It is evident from this discussion that to provii all of these precision indexes would make this section unnecessarily long and impair its usefulness. The decision i how many of the possible indexes are to be included in a t method is left to the discretion of those who formulate ai use the test method. In this practice, however, the pi ecisii statement is based on the two indexes --repeatabiliu <ir reproducibility as defined in 3.26: Precision of Test Method--In an interlaboratory study of this t( method in which____operators in_____laboratories tested _ coatings with a broad range of____ (property) levels (analyzed__ materials containing__ _), the intralaboratory standard deviatii (coefficient of variation) was found to be____ units (percent) wi --_ degrees of freedom (df) and the interlaboratory stands deviation (coefficient of variation)____ units (percent) with____ after rejecting____ results(s) from____ laboratory (ies) for one tit because the range between replicates (repeats) differed significant from all other ranges for material ____, or all results from o laboratory for material____because the mean differed sigmlici' I froth all other means. Based on these standard deviations (cod dents) the following criteria should be used forjudging, at the 95 confidence level, the acceptability of results: Repeatability--____results, each the mean of_____ replicates applicable), obtained by the same operator should be considet<ffi{ suspect if they differ by more than____units (% relative). Reproducibility--Two results, each the mean of____ replicatst obtained by operators in different laboratories should be co-w c-iCJ - suspect if they differ by more than____units {% relative). N' 6--Where the results obtained are in percent instead of some) unit add "absolute" after X % in the repeatability and reprodudbiii$l statements to distinguish from cases where use of the coefficients QWf, variation results in percent relative precision limits. N' 7--Users of ASTM test methods should he aware that precision obtained from an interlaboratory study is for measunaneaSg made on the same batch of each material. Consequently, nonr.ah* batch-to-batch variability, which is governed by manufacturing qualify control, is not included in the precision values established for a tc$i| method. 628 D UP05 0297810 D 3980 ANNEX (Mandatory Information) AI. Discussion of Table 10 JH Two points are evident: (I) neither the intralab- nor interlaboratory variances can be pooled because fptdard deviations increase with higher hardness values; |lp intralaboratory coefficients of variation are homogeH*..; but there is one discordant value (Enamel E) in the ^jgjUtibratory coefficients. "Tift~ bVj t The tests referred to in 15.1.1.4 can be applied to that the interlaboratory coefficients cannot be mljk or, as shown below, the coefficients are pooled to Hpne: if any maximum allowable difference is then "Bid. Pooling the coefficients of variation in accordance me formula in 15.1.1.8 yields the following: A1.4 The interlaboratory coefficients of variation are now all homogeneous so they can be pooled with total degrees of freedom of 58 for intralaboratory and 23 for interlaboratory coefficients. P . . = [5(127.1548) + 4(35.1667)j`/l = /776.4403SVA E V" [ {5 X 5) + (1 x 4) J { 29 / = (26.7738)4 = 5.174 %; = 17.65 % for three determinations. JPooled vb = '5(714.9841) + 4(119.6289)T/J = 25 + 4 = (139.7737)'* = 11.82 % >f tLe1*; irovidc t sec%Jl >ion on* 'i a i test' ite and rcisLOn ty aiiS his.tekjR *vu-t dm Me?; Lt) v, th andaifSfi * (It | ficates, = (25.5479),/= = 5.055 %. ft"|r three determinations vw- cj> = 5.055 x 3.40 = 17.19 ' k....P...o..o..le..d. vb = /^1--4--]-1-.-8--3-6--4- j\'/1 = (235.3061)'* = 15.34 5 |Porfive laboratories v?= 15.34 x 4.17 = 63.97 %. jjeicfore the acceptable range for Enamel E is 0.172 x = 1.94 for intralaboratory results and 0.64 x 11.26 = lifer interlaboratory results. The actual maxima obtained h. Snamel E in the round robin are for the intralaboratory 11.3 for Laboratory It, and for the interlaboratory range between Laboratories I and IV. Thus, while the results Laboratory IV for Enamel E could not be rejected in |i 3.5 on the basis of Enamel E alone, they can be on the bf all six enamels. W.3 Instead of rejecting the results from all laboratories fie material, it is preferable to discard only those of the i ent laboratory. When this procedure is followed_for namel E the revised values are: ~ZX - 120.0, n = 12, X = SA2 = 1213.58, (2Xfjn = 1200, net total ss = 13.58, = 1210.7667, net laboratory ss = 10.7667, ifalaboratory ss = 2.8133, df = 8, sw2 -- 0.3517, sw = 0.593, : 5.93 %, interlaboratory df = 3, mean square = 3.5889, S = 3.2372, sL2 = 1.0791, >w 2/r = 0.1172, sb2 = 1.1963, : 1.09, v,, = 10.94 %. Rejecting one laboratory's results for one material reduced the pooled interlaboratory coefficient of variation from 15.34 % to 11.82%, which is certainly justification for discarding those results. A 1.5 From the pooled coefficient of variation the max imum acceptable difference, vb # is 34.4 % for two laborato ries, 46.4 % for four laboratories, and 49.5 % for five laboratories (Note A 1,1). Based on these values, the accept able range in Knoop hardness results for each enamel is given in Table Al .1 and compared with the maxima found in the study. N' A 1.1--The MAD used for determining the acceptability of results in the round robin must be based on the number of participating laboratories while that used in the final precision statement is for two laboratories. TABLE A1.1 Knoop,Hardness Ranges For Enamels Intralaboratory Interlaboratory Calculated Found Calculated Found A 0.22* 0.2 0.62 * 0.4 B 0.51 0.4 1.44 0.73 C 0.89 0.6 2.5 1.63 D 1.3 0.8 3.64 2.33 E 1.8 1.3 4.64 s 2.57 s F 3.0 1.7 8.3 4.83 A These values are smaller than in Table 9 because the precision estimate is better from ail six enamels than from Just one. 8 For four laboratories. f SOl&b nts of iat the imen^s (| lormal juality & tt 629 DUP050297811 #> D 3980 APPENDIX (Nonmandatory Information) (1) ASTM Manual for Conducting an Interlaboratory Study of a Test Method. ASTM STP 335, ASTM, 1963. (2) ASTM Manual on Quality Control ofMaterials. ASTM STP 15, ASTM, 1951. (3) ASTM Practice D 1749, for Interlaboratory Evaluation of Test Methods Used with Paper and Paper Products, Annual Book of ASTM Standards, Vol 15.09. (4) ASTM Practice D 2904, for Interlaboratory Testing of Textile Materials, Annual Book ofASTM Standards, Vol 07.01. (5) ASTM Practice E 173, for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals, Annual Book of ASTM Standards, Vol 03.05. (6) ASTM Practice E 691, for Conducting an Interlaboratory Test Program to Determine the Precision of Test Methods, Annual Book ofASTM Standards, Vol 14.02. (7) Bennet, C. A., and Franklin, N. L., Statistical Analysis in Chemistry and the Chemical Industry, John Wiley and Sons, New York, NY, 1954. (8) Brownlee, K. A., Industrial Experimentation, Chemical Pub lishing Co., 1947.. (9) Davies, O. L., Design and Analysis of Industrial Experiments, Hafner, 1954. (10) Finkner, M. D., '`The Reliability of Collaborative Tests for AOAC," Journal, Association of Official Agricultural Chemists, Vol 40, 1957, p. SS2. (11) Freeman, H. A., IndustrialStatistics, John Wiley and Sons, New York, NY, 1942. (12) Kempthome, O., Design and Analysis of Experiments, John Wiley and Sons, New York, NY, 1952. (13) Mandel, J., and Lashof, T. W., "The Interlaboratory Evaluation ofTesting Methods," ASTM Bulletin, No. 239, July 1959, p. 53, (14) Mandel, J., ed. Interlaboratory Testing Techniques, American Societyfor Quality Control, 1978. (15) Mandel, J,, "The Measuring Process," Technometrics, Vol 1 1 No. 3, 1959, p. 251. ' ] (16) Mann.H. B,, Analysis andDesign ofExperiments, Dover, 1949, (17) Natrella, M. G,, "Experimental Statistics," NBS Handbook 91? 1963. (18) Quenouille, M. H., The Design and Analysis of Experiments^ Hafner, 1953. (19} Youden, W. J., "Graphical Diagnosis of Interlaboratory Test! Results," Industrial Quality Control, Vol XV, No. l 1, 1959, p/J 28. The American Society ior Testing andMaterials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if hot revised, eWiar reapproved qr withdrawn. Your comments are Invited either for revision of this standard or lor additional standards and should be addressed to ASTKt Headpuarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may ettend. if you feet that your comments have not received a fair hearing you shoutd make your views known to the ASTM Committee.on Standards, 1916 Race St., Philadelphia, PA 19103. 630 DUP050297812 Designation: D 4017 - 90 Standard Test Method for Water in Paints and Paint Materials by Kail Fischer Method1 This standard is issued under the fixed designation D 4017; the number immediately following the designation indicates the ycaT of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year ofIasi reapprovai. A superscript epsilon () indicates an editorial change since the last revision or reapproval. til This test method is applicable to all paints and paint ffi'rials, including resins, monomers, and solvents, with the Sjjkion of aldehydes and certain active metals, metal |s, and metal hydroxides. While the evaluation was TJed to pigmented products containing amounts of water jp 30 to 70 % range, there is reason to believe that higher i|t lower concentrations can be determined by this test iffiiod. ] 2 This standard does not purport to address ail of the my problems associated with its use. It is the responsibility "p? user ofthis standard to establish appropriate safety and iyggh practices and determine the applicability ofregulatory Hations prior to use. Specific hazard statements are given (fiction 7. Referenced Documents Ip', ASTM Standards: .1193 Specification for Reagent Water2 ^ H I 80 Practice for Determining the Precision of ASTM ' Methods for Analysis and Testing of Industrial Chem- fflcals3 *|E 203 Test Method for Water Using Karl Fischer Reagent3 feummary of Test Method 3il The material is dissolved in pyridine, or another .appropriate solvent, and titrated directly with standardized Kail Fischer reagent, to an electrometric end point. The pgjish reaction with water in pyridine is accelerated with a hcmical catalyst, 1-ethylpiperidine. *`3.2 Pyridine is used as a solvent to minimize interference .rnhiems caused by ketones. It is also used because the more "omrikm solvent, methanol, will not dissolve many common resins, and because methanol reacts with some resins to Induce water. Jr 4 Significance and Use 1 4 l Control of water content is often important in control' "% the performance of paint and paint ingredients, and it is Jtical in controlling volatile organic compound (VOC) ntent. A,2 Paint materials are often insoluble in common Karl 'scher solvents such as methanol. Pyridine has been found 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint 'vd Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.21 on Chemical Analysis of Paints and Paint Materials. .Current edition approved May 25, 1990. Published July 1990. Originally |p^blished as D 4017 - 81. Last previous edition D 4017 - 88. 2 Annual Book ofASTM Standards, Vols 06.03 and l KOI. 3 Annual Book ofASTM Standards, Vo! 15.05. to be a nearly universal solvent for these materials; however, the Karl Fischer reaction is too slow in that solvent at room temperature. To speed it up, 1-ethylpiperidine is added at 5 % as a buffer, or "catalyst". 5. Apparatus 5.1 Karl Fischer Apparatus, manual or automatic, encom passed by the description in Test Method E 203. Apparatus should be equipped with a 25-mL buret, Class A, or equivalent. 5.2 Syringe, 100-p.L capacity, with needle. 5.3 Syringes, 1-mL and 10-mL capacity, without needle, but equipped with caps. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.4 Other grades may be used, provided it is ascertained that the reagent & of sufficiently high purity to permit its use without lessehing the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent grade water conforming to Type II of Specification D 1193! 6.3 Karl Fischer Reagent.5 6.4 Pyridine. 6.5 1-Ethylpiperidinef 6.6 Hydrochloric Acid (HC1), concentrated. N ' I--All reagents must be fresh. Do not use reagents, that are more than 9 months old. Karl Fischer reagent deteriorates .with age. Check expiration dates on the reagent bottle. 7. Hazards 7.1 Karl Fischer reagent contains four toxic compounds, namely iodine, sulfur dioxide, pyridine, and methanol or glycol ether. The reagent should be prepared and dispensed in a hood. Care must be exercised to avoid inhalation or skin contact, Following accidental contact or spillage, wash with large quantities of water. 7.2 Pyridine and methanol solvents should be treated with 4 "Reagent Chemicals, American Clicmical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY and the "United States Pharmacopeia." 5 SO-K.-3 available from Fischer Scientific Co., or equivalent has been found suitable for this purpose. 6 Use l-ethylpiperidine, manufactured by the Aldrich Chemical Co., Milwaukee, wr 53233, For the best results, 631 DUP050297813 # D 4017 Expected water, % 0.5-1.0 1-3 3-10 10-30 30-70 >70 TABLE 1 Specimen Guidelines Approximate Specimen Weight, S 5 2-5 1-2 0.4-1.0 0.1-0.4 0.1 Approximate Tilrant Volume at 6 mg/mL titre, mL 5-10 10-20 10-20 20-25 15-25 20 the same care as Karl Fischer reagent 7.3 1-ethylpiperidine is of unknown toxicity and, there fore, should be handled with the same care as the materials listed in 7.1 and 7.2. 8. Procedure 8.1 Standardization ofKarl Fischer Reagent: 8.1.1 Add enough fresh pyridine to cover the electrode tip, plus 1 mL of 1-ethylpiperidine catalyst per 20 mL of pyridine. Catalyst performs best at a concentration of about 5 % of the volume present. 8.1.2 Fill the 100-pL syringe to about half full with distilled water and weigh to the nearest 0.1 mg. 8.1.3 Pretitrate the pyridine to the end point indicated by the equipment manufacturer, by adding just, enough Karl Fischer Reagent 1 (KFR) to cause the end point to hold for at least 30 s. 8.1.3.1 The use of the catalyst greatly increases the reac tion rate between water and Karl Fischer reagent. To obtain reliable results, increase the electrode sensitivity and reduce titration rate to a minimum. Most instruments have controls for these functions. Consult the instructional manual for information on these controls. 8.1.4 Empty the contents of the syringe into the titrator vessel. Immediately replace the stopper of the sample port and titrate with KFR to the end point as described in 8.1.3. 8.1.5 Repeat standardization until replicate values of F agree within 1 %. Determine the mean of at least two such determinations. Carry out calculations retaining at least one extra decimal figure beyond that of the acquired data. Round off figures after final calculations. 8.1.6 Calculation: 8.1.6.1 Calculate the KFR titre F as follows: F-J/P (1) where: J = water added, g, and P = KFR used, mL. The value for F should be recorded to the four significant digits and should be the mean of at least two determinations. Typical values are in the range of 0.004000 to 0.006000 g/mL. 8.2 Analysis ofSamples With More Than 0.5 % Water. 8.2.1 The titration vessel should already contain preti trated pyridine and catalyst, as described in 8.1.1 and 8.1.3 in the standardization procedure. Best results are obtained with fresh solvent, that is, containing no previously titrated specimen in the vessel. 8.2.2 With a 1-mL or 10-mL syringe, draw the amount of material indicated in Table 1. N' 2--Paint samples tend to settle in the syringe and give bjpj, percent water content. Obtain a freshly stirred or mixed specimen f0r : each test run. 8.2.2.) Remove the syringe from die specimen, pull the plunger out a little further, wipe the excess material off the syringe, and place a cap on the syringe tip. Weigh the filled J syringe to the nearest 0.1 mg. 8.2.3 Remove the cap, and empty the syringe contents < into the pretitrated pyridine vessel. Pull the plunger out and . replace the cap. 8.2.4 Stir rapidly for 1 to 2 min before starting titration: I Some instruments can be set to do this automatically. If the j specimen is still not dissolved or dispersed, continue stirring ' until it is dissolved, or use a different solvent in place of pyridine in 8.2.1. 8.2.5 Titrate the specimen slowly with KFR to the end point described in 8.1.3. 8.2.6 Reweigh the emptied syringe, and calculate the specimen weight by difference. 8.2.7 Calculation: 8.2.7.1 Calculate the percent water L as follows: I = (fxFx 100)/S (2)' 8.3 Analysis ofMaterials With Less Than 0.5 % Water. 8.3.1 For 0.1 to 0.5%, follow procedure in 8. specimen), except substitute a 1-mL microburet for the3 25-mL buret in the Karl Fischer apparatus. 8.3.2 For less than 0.1 %, use a 1-mL microburet and J increase specimen size as much as needed, up to 10 g. It should be possible to measure moisture levels down to 1 ppm (0.0001 %) by this approach. N' 3--Specimens with less than 0.1 % water may require sp-'i.l handling techniques to prevent pickup of atmospheric moisture. Tlrasf precision of this test method 'was determined with specimens containing . higher water levels. 9. Recommendations for Good Results 9.1 Make sure electrodes are clean. 9.2 Follow manufacturer's instructions to ensure that venting into the titration vessel is only through a dessicant^ 9.3 Samples should be thoroughly mixed before taking a , specimen. 9.4 Paints and paint materials are often slow to dissolve . disperse. To ensure that all of the water is extracted into i pyridine or solvent, stir rapidly for 1 or 2 min before star the titration. 9.5 Run the titration slowly with rapid stirring. 9.6 Throw out the first result in fresh pyridine. 9.7 Use only Aldrich's 1-ethylpiperidine.6 It has been, found that other brands produce variable results. ''ill! 10. Maintenance 10.1 Cleanup--Clean the titration vessel by rinsing with fresh pyridine. Do not use methanol or other solvents. 10.2 Dryness--Check frequently to be sure that all drying tubes are in good condition and tightly connected. Replace dessicant when indicator color changes through half oj the ' tube. 10.3 Electrode Performance--If electrode response is slug gish or otherwise off standard, take the following steps u' turn, to correct the problem. Test the electrode with a 632 DUP050297814 1 gi'T liPh semen fop pull the tl off the the filled. conic nis out and;: titration, ly. ifthe;; stirting place 0f the ena;i late the (tr Water i.2 n-g,.;t for thet tel arte10 ?. lit ,) I npmf e speq^Mj ure. nta.nxiiE, la D 4017 -tilion after each step, to determine if the next step is uired. f.0.3.1 Wipe the electrode tip with a clean paper towel. jo.3,2 Wash the electrode by dipping in concentrated Irochloric acid for at least 1 min. Rinse first with distilled ^er, then with methanol. Ij 0.3.3 Follow manufacturer's instructions on resetting d point meter. 10.3.4 Replace power source. See manual for replacement Scedure. 10.3.5 Replace the electrode. Piecision and: Bias .1. The precision estimates are based on an interifatory study in which one operator in each of seven creht laboratories analyzed in duplicate oh two different fseven samples of water-based paints of various types dining between 25 to 75 % water. The results were analyzed statistically in accordance with Practice E 180. The within-laboratory coefficient of variation was found to be 1.7 % relative at 98 df, and the between-laboratory coeffi cient of variation was 5.3 % relative, at 42 df. Based on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level. 11.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 4.7 % relative. 11.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 15.0 % relative. .11.2 Bias--Bias has not been determined for this test method. 12. Keywords 12.1 Karl Fischer reagent method; moisture content; water content The American Society for Testlngand Materials fates no position respecting the validity of wry patent rights asserted in connection with any item mentioned in this standard. Users ofthtesiandard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of auoh rights, ere entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invitedeither for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive carefui consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your viev/s known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. urnm* n *j g wjtfjlg diyjiy,1 S-.U p. in l vilh a 633 D UP 050297815 Designation: D 4039 - 87 Standard Test Method for Reflection Haze of High-Gloss Surfaces1 This standard is issued under the fixed designation D4039; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (*) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method describes a procedure for using two specular gloss measurements to obtain a haze index for high-gloss nonmetallic specimens (1-4).2 It is particularly useful for evaluating the haze in clear finishes on nonglossy substrates, and the haze in reflected images produced by the surfaces of opaque glossy pigmented finishes. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 523 Test Method for Specular Gloss3 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D 3964 Practice for Selection of Coating Specimens for Appearance Measurements3 3. Terminology 3.1 Definitions: 3.1.1 specular gloss--the relative luminous reflectance factor of a specimen at the specular direction. 3.1.2 reflection haze--perceived cloudiness in an image reflected by a glossy surface. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 60* specular gloss--specular gloss measured with the 60geometry specified in Test Method D 523. 3.2.2 20 specular gloss--specular gloss measured with the 20 geometry specified in Test Method D 523. 3.2.3 haze index. H--a measure of reflection haze, where H = (Gfi0 - G> ); Ge0 is the 60 specular gloss and G2o is the 20 specular gloss. 4. Summary of Test Method 4.1 Measurements of 60 and 20 specular gloss are made on a specimen. The haze index is computed as the difference between the two measurements. 1 This lest method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.26 on Optical Properties. Current edition approved June 26, 1987. Published August 1987. Originally published as D4039 - 81. Last previous edition D 4039 -81. 2 Boldface numbers in parentheses refer to the list of references at the end of this test method. 3 Annual Book ofASTM Standards, Vol 06.01. 4.2 This test method is applicable to nonmetallic spu-. mens having a 60 specular gloss value greater than 60 m accordance with Test Method D 523. 5. Significance and Use 5.1 Haze is produced by irregularities in the reflect m surface that affect the distribution of flux reflected around the specular angle. The procedures specified in Test Method D 523 are not designed to measure reflected-flux scatter iy characteristics of high-gloss finishes, particularly where spec imens having different surface refractive indexes are being compared. A better index of scattering can be obtained hi making two specular reflectance measurements, that is, the use of two receptor apertures of different size. 5.1.1 In this test method, values for reflection haze are obtained from two measurements of specular gloss, < re made with a large receptor aperture and the other made with a small receptor aperture. The geometric conditions have been chosen to permit the use ofglossmeters that provide specular gloss measurements (large receptor aperture) and 20 specular gloss measurements (small receptor aperture) as specified in Test Method D523. 5.2 Measured gloss values of specimens depend on the , angle of illumination, refractive index of the material, and j the geometric distribution of the reflected light. The gloss scale ofboth the 60and 20 geometries is defined as 100 for polished black glass with a refractive index of 1.567. How ever, the polished black glass standards used in this lest 1 method usually have a tower refractive index (approximately ,, 1.53). Therefore, they will have a gloss value less than ti u These gloss values will be different for 60 and 20 measure-,' ments. Ifthe refractive index is 1.53, the black gloss stand;nJ will have a 60 gloss value of approximately 94 and a 20' gloss value of approximately 89. Therefore, this haze-fred* standard will have a haze index value of 94 - 89 = 5. A`K haze-free coating (refractive index of approximately 1.53)':j will have a corresponding haze index of 5 units, the difference between its 60 and 20 gloss values. Because 20 gloss changes much more rapidly with index than 60glo.s, the reflection haze value of a specimen also depends on tbe` index of refraction of the material. To establish a correction for the effect of refractive index would require measurement of the index for each specimen, which is impractical. Comparisons of reflection haze evaluated by this test method are therefore limited to specimens of essentially the same refractive index. 6. Apparatus 6.1 Glossmeter(s) capable of measuring 60 and 20 specular gloss in accordance with the specifications given in Test Method D 523. 634 DUP050297816 Preparation and Selection of Test Specimens .1 This test method does not cover preparation techues. When a test requires the preparation of specimens |n a liquid coating, specify the techniques of specimen paration. |2 Select test specimens in accordance with Practice 3964. 2.1 To determine the maximum gloss obtainable from a erial, such as a paint or a varnish, use methods in Test ods D 823 to produce a film of uniform thickness on a 6th, planar substrate. 2.2 Use surfaces of good planarity, because surface ;e, waviness, or curvature may affect test results cantly. The directions of brush marks or similar re effects should be parallel to the plane of the axis of two beams. Calibration and Standardization 1 Calibrate the glossmeters with primary and secondary king standards in accordance with the procedures given Lest Method D 523. Procedure 9.1 Select an area near the center ofthe test specimen and Sermine the 60 specular gloss. ,9.2 Determine the 20 specular gloss on the same area of lie specimen. 1 Calculation 0.1 Compute the haze index, H, as follows: I " Gso " G2" where: G60 = value of 60 specular gloss and G2o = value of 20 specular gloss. N' I--Because of the difference in the assigned values for the black glass standard at 20 and 60", the haze index for specimens without haze will have value of approximately 5. 11. Report 11.1 Report the following information: 11.1.1 For each specimen, the measured G60 and G20 values and the computed haze index, H. 11.1.2 Where preparation of the test specimen has been necessary, describe or otherwise identify the method of preparation. 11.1.3 Identify the glossmeter used by make and mode). 11.1.4 Identify the gloss standards used. 12. Precision 12.1 On the basis of interlaboratory studies of this proce dure in which six laboratories conducted single determina tions on eight high-gloss coatings differing in visually per ceived reflection haze, the within-laboratory. standard deviation for haze index values was found to be 0,9, and the between-laboratories standard deviation was found to be 2.5. 12.2 Based on these standard deviations, the following criteria should be used for judging the acceptability of single determinations at the 95 % confidence level. 12.2.1 Repeatability--Two results obtained by a single operator should be considered suspect if they differ by more than 2 units of haze index. 12.2.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than 7 units of haze index. REFERENCES jlNimeroff, I., "Two-Parameter Gloss Methods," Journal of RejSearch, National Bureau of Standards, Vol 58, No. 3, March 1957, ?p. 127-135. Pammond, HI, H. K., and Nimeroff, I., "Measurement of Sixtyipegree Specular Gloss," Journal ofResearch, National Bureau of ^Standards, Vol 44, No. 6, June 1950, p. 585. (3) Horning, S. C., and Morse, M. P., "The Measurement of the Gloss of Paint Panels," Official Digest, Federation of Paint and Varnish Production Clubs, March 1947, p. 153. (4) Hunter, R, S., "Gloss Evaluation of Materials," ASTM Bulletin, No. 186, December 1952, p. 48. (5) Hunter, R. S., The Measurement of Appearance, WileyInterscience, New York, NY, 1975. The American Society for Testing endMaterials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of Infringement of such rights, are entirely their own responsibility. This standard ts subfect to revision at anytime by the responsible technical.committee and must be reviewed every five years and it not ravised, either reapproved or withdrawn. Yourcomments are invited either lor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive Careful consideration at a meeting of the responsible technical committee, which you may attend. If you leal that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 635 DU PO 502 97817 Designation: D 4040 - 91 Standard Test Method for Viscosity of Printing Inks and Vehicles by the Falling-Rod Viscometer1 This standard is issued under the fixed designation D 4040; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {<} indicates an editorial change since the last revision or reapproval. 41 N' --Tables AM and A 1.2 editorially corrected and the year date changed to Nov. 15, 1991. 1. Scope 1.1 This test method covers the procedure for determining the falling-rod viscosity of printing inks, vehicles, and similar liquids that are essentially nonvolatile and unreactive under ordinary room conditions. 1.2 For printing inks, which are typically non-Newtonian, this test method is applicable in the apparent viscosity range of about 10 to 300 P at a shear rate of 2500 s-1. For Newtonian liquids, the applicable viscosity range is about 10 to 1000 P (I P = 0.1 Pa-s). 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8. 1 distance L over which a unit thickness x of the liquid is i stressed: D - LjxF. 1 3.1.4 Newtonian--refers to a liquid whose viscosity is' constant at all shear rates. 3.1.5 non-Newtonian--refers to a liquid whose viscosity varies with shear rate. Such liquids may be either shear- \ thinning (pseudoplastic) or shear-thickening (dilatant). Most. printing inks are shear-thinning. j 3.1.6 apparent viscosity, VD--the viscosity of a non-* Newtonian fluid at a particular shear rate D. A shear rate ofil 2500 s-' has been found useful for printing inks and is J specified in this test method. j 3.1.7 yield stress, Sa--the minimum shear stress require|fj to initiate motion in a non-Newtonian liquid. j 3.2 Description of Terms Specific to This Standard: t 3.2.1 power law--a mathematical model that presumes: that the viscosity of a liquid varies with shear rate in i accordance with a power function as follows: j 2. Referenced Document 2.1 ASTM Standard: D445 Test Method for Kinematic Viscosity of Trans parent and Opaque Liquids (and the Calculation of Dynamic Viscosity)2 kmj. k DN where: k -- a constant related to the viscosity of the liquid and | JN = a constant describing the rate at which shear stress! varies with sheaf rate. 3. Terminology The value of N is precisely 1,0 for a Newtonian fluid, less! than 1.0 for a shear-thinning liquid, and greater than 1.0 f|pj 3.1 Definitions: a shear-thickening liquid. ,I 3.1.1 viscosity, V--the ratio of shear stress to shear rate. 3.2.2 power law plot--a logarithmic plot of shear stress! The viscosity of a liquid is a measure of the internal friction versus shear rate based on the expanded form of the pow||| of the liquid in motion. The cgs unit of viscosity is 1 g/cm-s law equation: % (1 dyne-s/cm2) and is called a poise. The Si unit is 1 N-s/cm2 and is equal to 10 P. In S-'ink+N In D 3.1.2 shear stress, S--shearing force per unit area; the For liquids conforming to the power law, the fogarithmtaj unit is 1 g/cm-s2 (1 dyne/cm2). In the falling-rod viscometer, plot of S versus D is linear over the shear rate range Ig shear stress is proportional to total weight W per unit of interest. The slope of the line, is the power law constant At' ' shearing area A times the gravitational constant g, in 3.2.3 shortness--the property of a non-Newtonian fluiBlJ accordance with the equation: S = Wg/A. that prevents it from being drawn into a filament. 3.1.3 shear rate, D--velocity gradient through the stressed 3.3 Symbols (for Power-Law Calculations): liquid; the unit is 1/s or I s-1'. In the falling-rod viscometer, B = intercept of a straight line. shear rate is inversely proportional to fall time F per unit* 3 F = measured fail time, s. Fc = corrected fall time, s. ^2500 = fall time equivalent to a shear rate of 2500 s-1, s. 5 This lest method is under the jurisdiction of ASTM Committee D-l on Paint ^2500 = apparent viscosity constant at 2500 s"', cm"'s~'. and Related Coatings and Materials and is the direct responsibility of Subcom N = slope of the power law plot, a measure of non-j mittee DO 1.56 on Printing Inks. Current edition approved Nov. 15, 1991. Published January 1992. Originally Newtonianism, cm2/dyne-s. published as D4040-81. Last previous edition D 4040-89. SF = shortness factor, s_l. 3 Annual Book ofASTM Standards, Vol 05.01. S' = pseudo yield value, dyne/cm2 636 DUP050297818  4040 - measured specimen temperature, C. reference temperature, C. apparent viscosity at 2.5 s-1, P. apparent viscosity at 2500 s-!, P. total weight, g. - added weight, g. weight of rod, g. weight required to obtain a shear rate of 2500 s-1. jf' jjjpnmary of Test Method faK'This test method is based on measurements of the tKequired for a weighted rod to fall through an aperture mtjining the test specimen, `ffX Fall times are corrected to a reference temperature of 'tffbr other mutually agreed-upon temperature). The test .usfltpd specifies precise measurement of actual specimen |perature in order to detect fluctuations due to cooling by I, a e(al, heat of friction during shearing, and body heat of the Ifc.'tor. ' 3 Each specific instrument must be calibrated in order nfltablish the fall time that is equivalent to a shear rate of ' s'1. 14 Fall times as a function of weight are extrapolated to JbQI i s_1 by means of the power law (logarithmic) relation'll'p between shear stress and shear rate.' Apparent viscosity 2500 s-1 and the degree of non-Newtonianism are imined by calculation or graphically. The calculation of Sjcal low shear parameters is also covered. JSjgnificance and Use Mp Apparent viscosity at the relatively high shear rate of s-1 does not completely define the rheological properill of printing inks but is useful in the practical control of gViscoSity during production and the specification accep- le between supplier and purchaser. _ 5.2 The slope of the power law plot is the preferred |i|asure of non-Newtonianism. The yield value, which is btained by extrapolation of high-shear measurements to a hlar rate approaching zero, does not conform to the efinition of the true yield stress (see 3.1.7). The yield value Ind bther low shear parameters are also Subject to a high leglfee of variability (see the precision table in Section 16). 'Apparatus 6.i Fall-Time Runs: (iig.l.l Falling-Rod Viscometer? equipped with a swinging pplatform and automatic timing device34 accurate to at least i,l s, preferably 0.01 s. A special lightweight rod is useful for pUiquids in the 10-P range. " 6.1.2 Set of Tapped or Slotted Weights--Weights of 50 or s 100 to 500 g are usually provided with the instrument. Extra 500-g weights, approximately 4, totaling about 2000 g are required to handle fluids at the upper end of the practical JUS'uf-r iJ&l 3 Commercial units include the Laray Viscometer available from Testing Machines. Inc., 400 Bayview Ave., Amityville, NY 11701; Thwing-Albert Model LR from Thwing-Albert Instrument Co., 10960 Dutton Rd., Philadelphia, PA 19154; Churchill from Churchill Instrument Co., Ltd., Greeuford, England. 'Platform and timing device are standard on newer viscometer ..models. For equipping older models, see Bassemir, R., "Evaluation of the Laray Viscometer," ; American Irik Maker, Vol 39, No. 4, April 1961, pp. 24-26 and 60. range. A 25-g weight is useful for liquids in the 10-P range. 6.1.3 A Thermostatically Controlled Cabinet, optional (if room conditioning is not available). Alternatively, a special collar5 through which water is circulated from a constanttemperature bath. 6.1.4 Thermistor,6 equipped with a probe having a re sponse time of 3 to 6 s. 6.1.5 Ring Stand and Clamp, or Other device for holding the thermistor probe in a suitable position. 6.1.6 Small Plastic Spatula--Metal spatulas are not suit able. 6.1.7 Plastic Scraper, consisting of a piece of flexible plastic, approximately 30 by 70 mm, having a semicircle cut out at one end; semicircle should fit the rod. 6.2 Instrument Calibration: 6.2.1 Balance, weighing to 0.1 g. 6.2.2 Metric Rule or Scale, at least 100 mm in length. 6.2.3 Vernier, Caliper, accurate to 0.01 mm, having a capacity of at least 30 mm. 6i3 Graphical Solutions: 6.3.1 Chart Paper, logarithmic 2 x 2 to 2 x 3 cycles.7 8 6.3.2 Triangle, 45, with a hypotenuse length of at least 100 mm (approximately 8 in.). 6.3.3 Protractor. 7. Materials 7.1 ASTM Standard Viscosity Oils? a minimum of two, preferably three, spanning the practical range of the fallingrod viscometer (used for calibration purposes only). 7.2 Lithographic Varnish or similar vehicle having a Viscosity of about 200 P.: 7.3 Lint- and-Metal-Free Rags or Tissues, 7.4 Naphtha or other low-boiling solvent in a wash bottle or closed metal container. 8. Hazards 8.1 Safety Precautions---Since solvents may be hazardous to the skin and eyes, in addition to other precautions, wear rubber gloves and safety glasses during cleanup to avoid solvent contact with skin and eyes.. In case of contact, wash skin with water; flush eyes for 15 min with water and call a physician. See supplier's Material Safety Data Sheets for further information on each solvent used. 8.2 Instrument Cautions: 8.2.1 Avoid any operation that will scratch the rod. Do not use a metal spatula. Never drop the rod through an empty aperture. 8.2.2 Weight loads in excess of 3000 g may cause bending of the rod. 3 Collars are available as accessories from (he respective manufacturers. 6 Suitable thermistors include Tele-Thermometer Model 43TA, with Model 423 probe from Yellow Springs Instrument Co., Inc., Box 279-T, Yellow Springs, OH 45387; and Model TSB with Model TP-7P probe from TRI-R Instruments Inc., 48 Merrick Rd., Rockville Centre, NY 11570. 7 Suitable chart paper includes Keuffel & Esser Nos. 46-7200 (22), 46-7280 (22.7), 46-7320 (23), all 8'Axl 1 green drawing; also available in green or orange tracing or 11x1616. 8 Certified standard viscosity oils are available from Cannon Instrument Company, P.O. Box 16, State College, PA 16801. Table 3 in Test Method D 445 shows satisfactory oils including S-600 (16 Pat 25'Q, S-2000 (57 P), S-8000(220 P), and S-30 000 (750 P). Viscosity at various temperatures is indicated on the label of each container. 637 DUP050297819 # D 4040 8.2.3 To minimize heat buildup from body temperature during a run, avoid contacting the viscometer block with bare hands. When instructions call for holding the block steady, wear a glove or place a small cloth in the palm of the hand. 8.2.4 When making fall-time measurements, work quickly and without interruption so that the entire run is completed within 5 to 10 min. N' 1--Many modern printing inks and vehicles contain some solvent, and volatile loss during a run can seriously bias test results unless rigorous control ofexposure time is exercised. Volatile loss can be detected if successive drops of the rod with the same weight result in increasingly longer fall times. 9. Preparation of Apparatus 9.1 Set the viscometer on a sturdy bench located in an area free of direct drafts, direct sunlight, and other sources of heat. Level the viscometer by turning the adjustable feet up and down until the spirit level bubble is centered. 9.2 Pass a hand over the upper and lower photocells to assure that the timer is activated and deactivated. 9.3 Attach the clamp to the ring stand and place next to or behind the viscometer. Drape the thermistor probe over the clamp; reset the clamp so that the probe end fils close to the viscometer block. 9.4 Clean the block and rod thoroughly with tissues wetted with naphtha. Remove residual solvent with clean dry tissue. Roll the clean dry rod over a flat surface to check for straightness. If rod is bent, discard and obtain a new rod/orifice set. . 9.5 Examine the markings at the ends of the rod. Select one marking as an indication of the "proper" end to be always inserted into the aperture first. 10. Calibration 10.1 Determine instrument constants in accordance with the procedure given in Annex Al. 10.2 Optional--If a graphical method is to be used for direct conversion of test results to viscosity, prepare Master Sliding Scale Calibration Graph as in Annex A2. 10.3 Periodically check calibration as in Section A 1.2. 11. Sample Preparation 11.1.1 Transport the sample to the test area and preserve in a closed container. Skin paper should be used for oxidative drying inks. 11.1.2 Ink samples should be uniform dispersions. If pigment settling is suspected, insert a spatula in the container and gently stir. Be careful not to introduce air bubbles. 11.1.3 Prior to the run, a portion of the sample may be transferred to a slab and gently spread out in order to remove bubbles, skin, or other debris. N' 2: Caution--Do not work the sample vigorously, this practice causes a significant increase in sample temperature. Be sure to close the container immediately after removing the desired portion.12 12. Conditioning 12.1 The temperature of the room {cabinet or collar) should be set at 23 1C (or 2"C below the reference temperature). N' 3--In accordance with Note 8, the allowable range f0 specimen temperature is 2aC from the reference temperature. How ever, during the coutse of testing, heat of shearing and body heat of the operator both contribute to continuous temperature rises in (jjjf specimens, notwithstanding room, cabinet,,or collar conditions. Xq : allow for inevitable temperature rises, temperature controls are set at thj lower end of the allowable range. ' 12.2 Equilibration of test samples is not necessary. Specimen sizes are small (less than 2 mL); when spread out on if slab and applied to the viscometer, both hot and cold samples quickly reach the temperature of the metal. 12.3 If the viscometer has been idle for more than an hour, it may be necessary to bring it into equilibrium with, the conditioning temperature (23C or other specified in' 12.1). Make preparations for an exploratory run (13.2 to 13.5) using a varnish if the test specimen contains volatiles. Read specimen temperature; if too low (a possibility considering that metal serves as a heat sink), add a 1000-g weight ! the rod and make a few drops (13.7 to 13.9 but without recording time) until the specimen temperature reaches thai: of conditioning. Continue the run or, if a varnish was used, clean up. 13. Procedure for Fall-Time Runs 13.1 If required, prepare, level, and condition the instrut. ment as described in 10.12.1 and 12.3. 13.2 With the proper end of the clean rod down; hold t rod vertically over the clean aperture and gently lower until it, f rests on the swinging platform. fiS13.3 Transfer a uniform specimen to the tip of a clean plastic spatula. The specimen size should be sufficient to the well of the viscometer. 13.4 Hold the rod with the fingertips and carefully raise about 20 .mm. Transfer the specimen from the spatula to the1! * rod as close as possible to the bottom of the well. Rotate the rod slowly to distribute the specimen around the well, ensuring that the well is full. Allow the rod to fall to the platform. 13.5 Place the thermistor probe in the well close to not touching the rod. The probe can remain in the well throughout the run. Turn the thermistor on. 13.6 Using experience or the information in Table 1 as a, guide, select a weight load, that will produce a fall time ^fl close to 1 or 2 s as is practical. N' 4--For comparison of non-Newtonian liquids, runs must not:!; be made at pre-specified rod weights. Rather, weights should be adjusted! to obtain pie-specified fell times, the first ofwhich corresponds as closely;) to a shear rate of 2500 s_I as is practical. 13.7 Hold the block level and steady with one hand (seSi 8.2.3). With the other hand, carefully place the selected weights on top of the rod. If weights are slotted, evenly distribute the slots around the circumference of the rod. Make certain that the rod is vertical. (If weights tend to make the viscometer unsteady, retain the hand on the block so that the rod falls smoothly in 13.8.) 13.8 Set the timer. Release the platform and allow the rod to fall naturally. If the fall time is within the desired range (for example, 1 to 2 s for the first weight, etc.), record the added weight fVA, fall time F, and specimen temperature T on worksheet. 13.9 Remove the weights from the rod. Pull the rod up 638 DU P050297820 # D 4040 aSE fo re. How. ;at of'hs ln <esl ' ions T0 J setaKhe ' Sp. . ut ci. a id cold han an m v iih fied 13.2 to ilatiles xinsidj-J sight to1 who it i es tut s used^S - : ..ii.'i instnir;r >Id the antifff tlea i florlll i raise tO.ftj#*,;^ ite tjisljJ Heir to the 'Ip 0 bin ; welt 1 asa-' no as ist not ;jj (justed >J ;Ic.sJ> ! (see ectal venly rod na w ithr.1 ;rod anuc I ihe ire T i up TABLE 1 Weight/Fall-Time Relationships for Newtonian Liquids A Rod weight = 130 g iffvfscosUv of J. fluid, P io 50 ip < * 250 TT 500 10Q0 1 200 1 300. 3 000 7 000 15 000 25 000 2 50 700 1 400 3 800 7000 18000? Fall Time, s 4 Added Weight, g 6 300 700 1 800 3 200 8 000 100 400 1 100 2200 5500 10 ft 50 150 700 1400 3000 20 25 300 600 900 iSfelghts required may be more or less depending on Instrument type and degree of wear. Printing inks will require additional weight depending on degree of ' organism. .`.'eights are impractical or. not recommended. . fly with the fingertips of one hand while holding the aineter block firmly with the other hand. Rest the rod on swinging platform. Using the plastic scraper; scrape the jjijr" of specimen from the top to the bottom of the rod s it enters the block. Gently rotate the rod in the weli to li (tribute the specimen. 3.10 Repeat the drop (13.7 to 13.9) with the same or djirated weights until two fall times with a specific set of - jilts agree within 2 % (0.04 s at a 2-s fall time, 0.2 at a fall time, etc.). l3sll Make additional measurements (13.7 to 13.10)with ecdingly lighter sets of weights, each approximately 50 % |e previous set, but do not exceed a fall time of 20 s. No ' 5--Newtonian liquids may be run with only one or two sets of agnts. Non-Newtonian liquids require at least four or five. fj.12 If the specimen is deplenished during the run, clean and start over from 13.1, preferably using ink fresh from Container. Make certain that the quantity of specimen is (listent. 13 13 Immediately after completing the run, turn the fiei n-istoroff. remove the probe from the well, and clean the p. e, the viscometer orifice, and the rod thoroughly. Nu.' S 6--Singe each test involves replicate fall-time measurements at Etc five weights, a single viscosity determination is usually considered (Ku.te. j|, Calculation ' 7---This section covers calculations by computer or program- &b(e calculator. The list of symbols is given in 3.3. The procedure for uphical solution of test results is described in the Annex A2. i 1.1 Enter into the computer the values for the instru- uent constants, WR, F2sa0 and ^2500 and the reference operature TK. ' '14 2 Enter data from fall-time runs in sets of Wh, `^plicate values of F that agree within 2 %, and the corre- ondmg values of T. 14.3 Compute the non-Newtonianism parameter N by limuUaneous solution of the following general equation: log W-- B -- N log Fa (1) "Mien.: W = WA + WR h.li (2) Fc = F + 0.1 F(T-Tr) (3) N' 8--Equation 3 corrects each measured fall time by 10 % per ^degree differential between the measured temperature and the reference temperature and is applicable only within 2`C of TR. As noted in the third column of Table A1.2, specimen temperature increases progres sively during a run. For accurate results, it is important that the temperature correction be applied to the fell time corresponding to each added weight. Otherwise, significaht error will bi introduced into the slope of the power law plot. 14.4 Examine (by computer) the value of N. Any value over 1.0 is improbable for a printing ink or a vehicle and suggests error in the test measurements; check data or repeat runs. Alternatively, treat any value between 1.0 and 1.05 as 1.0. 14.5 Compute the viscosity at 2500 s~' as follows: where: 1*2500 = ^25001*2500 (4) W2sao = antilog [B t N log F250a) (5) 14.6 Optional--Compute the viscosity at 2.5 s_l from either Eqs 6 or 7 as follows: V2.5 = *2500 (lOOO1-^) (6) or V2S = 1000 K&oo antilog {B - N log 1000 F2500) (7) 14.7 Optioml- -Compute the pseudo yield value as follows: S'0 = 2.5 (K, 5 - V25(j0) . (8) N' 9--Since the logarithmic nature of the power law precludes a zero shear rate, Eq 8 was derived to approximate the Bingham yield value, which is normally determined by extrapolating the linear portion of a shear stress/shear rate plot to zero rate of shear. 14.8 Optional--Compute the shortness factor as follows: SFS'JV25B0 (9) 15. Report , 15.1 Report apparent viscosity at 2500 s-1, degree of non-Newtonianism, reference temperature, and identifying code referring to the specific viscometer. 15.2 Optional--Report the viscosity at 2.5 s~', the pseudo yield value, and the shortness factor. 16. Precision 16.1 An interlaboratory study of this test method was conducted in which a single operator in each of nine laboratories made one run consisting of at least four repli cated data points on four inks on two different days. The inks ranged in viscosity from 10 to 300 P. The results were calculated on a single programmable calculator. One labora- 639 DUP050297821 D 4040 TA8LE 2 Precision of Falling-Rod Viscosity Determinations Test Results N ^2600 ^2.5 S',, SF Standard Deviation, % relative Degrees of Freedom Repeatability 3.3 5.4 11.5 14.6 17.7 4 4 4 3 3 Maximum Allowable Difference, % relative 7.6 15.3 31.4 41.2 50.1 N ^2500 ^2.5 S'. SF Reproducibllly 4.6 28 7.9 28 17.5 21 22.3 21 23.6 21 12.9 22.3 49.5 63.1 66.9 tory was a consistent outlier and was deleted from the entire analysis, and. the 10 P ink. was deleted from analysis of the low shear parameters. The estimated standard deviations and the degrees of freedom are given in Table 2. (Since the standard deviation was proportional to the test value, preci sion statements are made in terms of percent ofthe observed value.) Based on these standard deviations, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 16.1.1 Repeatability--Two results obtained by the same operator on different days should be considered suspect il they differ by more than the maximum allowable difference indicated in Table 2. 16.1.2 Reproducibility--Two results, each the mean of results obtained on different days by operators in differed laboratories, should be considered suspect if they differ b) more than the maximum allowable difference indicated in Table 2. 17. Keywords 17.1 printing inks; inks; vehicles; viscosity; apparent vis cosity; non-Newtonianism; yield value; power law viscosity: shortness; viscometers; falling-rod viscometers ANNEXES '(Mandatory Information) .1 Al. CALIBRATION OF FALLING-ROD VISCOMETERS A1.1 Determination ofInstrument Constants: Al.l.l Measure the distance between photocells of the timing device. Adjust to 100 + 0.5 mm. Divide ,by 10 and record as L in centimetres in chart patterned after Table AI.l. Al.1.2 Weigh the dean rod to 1 g. Record as WR. A1.1.3 Using a caliper, measure the diameter ofthe rod to 0.01 mm. Record as d in centimetres. A1,1.4 With the caliper, measure the length of the block over which the liquid is sheared (total height ofblock minus ink well) to 0.01 mm. Record as h in centimetres. Al. 1.5 Calculate apparent shearing area from the equa tion A = vdh. Record as A in square centimetres. N' AI.l--The shearing length of the block contains both a. .: tapered and a parallel section; therefore, it is understood that A is not the true shearing area but an apparent shearing area. A1.1.6 The thickness x of the test liquid is set by tic clearance between the aperture and the rod. Since the aperture consists of two radii, both of which are difficult to measure, a value for a mean gap clearance x can be Section Al.l.l Al.1.2 A1.1.3 A1.1.4 AI.l .5 AI.l.6 A1.1.7 AI.l .6 Symbol L wH d h A jr V g w Fc ^2500 t Editorially corrected. TABLE AI.l Instrument Constants for Falling-Rod Viscometers Definition bmed.fall distance (distance between photocells} weight of raa diameter of rod height of shearing portion of aperture apparent shearing area - tdh mean gap clearance viscosity of calibrating oil at reference temperature gravitational constant (approx. 980 cm/s2} total weight - rod weight + added weight corrected fall time fall time corresponding to shear rate of 2500 s-1 L/2500 a apparent viscosity constant al 2500 S'*1 K ,,6 2500A Unit cm g cm cm cm2 cm or pm P cm/s2 g s s cm-1 s"1 Typical values Laray ThwingAlbart 10.0 10.0 130 130 1.20 0.80 2.80 4.20 10.5 10.5 0.0045 45 0.0028 28 0.8 0.0372 1.4 0.0372 640 DUPO50297822 TABLE A1.2 Typical Worksheet for Falling-Rod Viscometer Run # GG32 Test sample Calibrating Oil S-200Q, V = 45.4 Instrument Laray LV #1 Reference temperature 25c^ Date of run 1-10-80 Rod weight 130 g Room temp. 22.8C Test Measurements Mean Results Corrected Results Recorded Fall Time F,S Specimen Temperature T.C Mean Fall Time* F.st Mean Specimen Tempre.racture* . Temperature Difference <r-25),*C Corrected Fall Timec Fa, s Total Weight0 W, g 1.45 24.49 1.55 24.55 1.59 24.66 1.57 24.61 -0.39 1.51 730 Newtonian Viscosity Multiplier^ WFC, g*s 1102 2.02 2.02 24.70 24.82 2.02 24.76 -0.24 1.97 530 1044 3.35 24.97 200 3.27 24.98 3.35 25.00 3.35 24.99 -0.01 3.35 330 1105 4.72 25.03 100 4.85 25.03 4.75 25.04 4.73 25.03 +0.03 4.74 230 1090 7.27 7.25 25.11 25.07 7,26 25.08 ping results only for fall times that agree within 2 %. fte number 25 refers to the reference temperature. Change figure if appropriate. |rmula: F,, = F 4- 0.1 F (f - 25).f J&Weight of rod plus added load. ^Complete this column only if sample is a calibrating oil or a Newtonian fluid. ' ^Editorially corrected. +0.08 7.28 155 1126 Mean WFC 1097 hipiited from fall-time runs on Newtonian, oils in the 'owing manner: A1.1.6.1 Using the procedure described in Section 13, Ire fail-time runs,on two" or three standard oils in random aucncc on two different days. Al 1.6.2 For each added weight, compute the mean of fall cs that agree within 2 %. Also compute the mean of the '^ponding temperature. Record as Fand Ton worksheet iffable A1.2). Correct each mean fall time according to (see 14.3). Record as Fc. 1,1,6,3 Take the sum of each added weight and the rod ht. Record as the total weight, W. }. 1.6.4 Multiply each total weight by the corresponding ected fall time and record as WFC. Examine trends in ^within each run. Values that change progressively with Pit are indicative of inadequate temperature sensing or ;Newtonianism in the oil. Check the source of error or eat with new oil if required. 1.1.6.5 Compute a mean WFC for each run and divide the viscosity of the oil at 25C (or other reference perature). The resulting values of VfWFc should be pttially the same for all oils. Compute the mean V/WFC. N' Al .2--If the label on the oil container does not list viscosity specifically at the reference temperature, the desired viscosity may be obtained from plots of log viscosity versus reciprocal of temperature on semi-logarithmic chart paper. Al.1.6.6 Compute the mean gap clearance x by multi plying V/WFC by AL/g. Record to three significant figures in centimetres (1CT4 cm = 1 pm). A 1.1.7 Calculate the fall time corresponding to a shear rate of 2500 s-1 from the equation: 11/2500 x. Record as F2500 in seconds to three significant figures. A 1.1.8 Compute g/2500 A and record as the "apparent viscosity constant at 2500 s_1," F250Cn in cm-s_l. A 1.2 Recalibration: A 1.2.1 Periodically determine several corrected fall times with one oil used for the original calibration. A 1,2.2 Calculate values for Wtc and compare with those originally obtained for the oil. Al.2.3 If the new values do not reasonably agree with the original ones, use the new fall time results to calculate a new value for the mean gap clearance x. Ifx increases by less than 5 % of the original value, the existing calibration may be retained. If the increase is between 5 and 20 %, repeat the entire calibration process. If gap clearance increases by 20 % or more, replace the rod and aperture. A2. GRAPHICAL SOLUTION OF VISCOSITY 1,2,1 Construction ofSliding Scale Calibration. Graph: chart paper, label the 2-cycle scale "Corrected fall time, s." A2.1.1 On a sheet of 2 by 2 to 2 by 3 cycle logarithmic (See Fig. A2.1.) Add one zero to the second cycle. Mark 641 DUP0502 97823 # D 4040 Viscosity at sa^c. piaa FIQ. A2.1 Typical Sliding Scale Calibration Graph position of F2500 (from A 1.1.7) on time scale. If below 1.0 s, the position can be located using another sheet oflog paper as a guide. Draw a horizontal line across the entire sheet of paper and label "2500 s-1 " at the far end. A2.1.2 Along the 3-cycle axis, mark the start of the cycles as 100, 1000, and 10000. Label the scale "Total weight, g" so as not to interfere with the line previously drawn for "2500 s'1." A2.1.3 Using the the results from fall-time runs made with standard oils (A 1.1.6.1) and found satisfactory in accordance with A1.1.6.4, plot corrected fall time versus total weight for each oil-day combination. Using the triangle, draw the best 45 line through the points so that each plot line intercepts the line labeled "2500 s'1." A2.1.4 From a second sheet of the same type of chart paper, cut a piece along the 3-cycle axis so that the resulting slrip contains the scale plus one or two graph divisions. Add zeros to the scale so that the second cycle starts at 10 and the third at 100; if required for high-viscosity fluids, a fourth cycle starting at 1000 may be obtained by pasting two strips together. Label the strip "Viscosity at 25C, P." Locate the 25C viscosity of each calibrating oil on the scale and draw vertical lines to the top. If three oils were used, there should be three lines on the strip. A2.1.5 Position the top of the strip directly beneath the 2500 s'1 line drawn on the first sheet of chart paper so that the viscosity lines on the strip match as closely as possible the intercepts at 2500 s'1. Paste securely in place. Cut off portions ofthe strip that extend beyond the edges of the chart paper. Relabel "Total weight" scale if strip hides pertinent coordinates. A2.1.6 The chart paper containing the viscosity strip represents the "Master Sliding-Scale Calibration Graph" for a specific instrument. Prepare an overlay containing the ,i desired identification information and paste in a suitable1 place (see example in Fig. A2.1). Make sufficient copies of, the master for normal use of the instrument. Be sure to preserve the original. N' A2.1--Use a duplication procedure that reproduces copy.. exactly. Office copiers and "quick" printing methods are prone to provide distorted copy. N' A2.2--The Master Sliding-Scale Calibration Graph is essen tially similar to the Inmont-Lehman chart, which is also based on,tot* power law but presumes that a shear rate of 2500 s'1 corresponds to a" * fall time of 1.0 s in all instruments. The charts issued by viscomisteiHt manufacturers are Cartesian {I IF versus W) and are based on Bingham.. A2.2 Graphical Solution of Viscosity: A2.2.1 Make the fall-time tun on the test sample ac cording to Section 13. Compute the corrected mean Lll times and the total weights according to A 1.1.6.2 and--Al. 1.6.3. A2.2.2 On a copy of the Master Sliding Scale Calibrator * Graph (Section A2.1), plot corrected fall time versus total, f weight for the test material. A2.2.3 Using the 45 triangle as a guide, check whether the best straight line through the plotted points is 45 greater to the weight axis. A line less than 45 is improbable for a printing ink or a vehicle and suggests error in the test measurements; check calculations or repeat the run. A2.2.4 Draw the best straight line through the points, making certain that the angle is at least 45to the weight axis Extend the line so that it intersects the horizontal axis at 2500 s'1. Read viscosity as the intercept on the sliding sea Record as K2500, apparent viscosity at 2500 s'1. A2.2.5 Center the protractor at the intersept and read the angle of the plot line. Subtract the measured angle from 90 and obtain the tangent from mathematical tables or a 642 DUP050297824 Ible calculator. Record as the non-Newtonianism paramiN. RjbTE A2,3--By turning Fig. A2.1 90 to the left, the graph can be lifted as a logarithmic plot of shear stress versus shear`rate, and the shear thinning nature ofthe test ink made more evident. The tangent of the angle with respect to the time (shear rate) axis is the power law constant /V. A2.2.6 Optional--Calculate V2A> 5"0, ancjt SF according to Eq 6 (see 14.6), Eq 8 (see 14.7) and Eq 9 (see 14.8). The American Society for Testing end Materials takes no position respecting the validity ofany patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years end Ifnot revised, either reapproved or withdrawn. Yourcomments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards-, 1916 Race St., Philadelphia, PA 19103. 643 DUP050297825 Designation: D 4060 - 90 Standard Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser1 This standard is issued under the fixed designation D 4060; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon.(c) indicates an editorial change since the fast revision or reapproval. 1. Scope 1.1 This test method covers the determination of the resistance of organic coatings to abrasion produced by the Taber Abraser on coatings applied to a plane, rigid surface, such as a metal panel. 1.2 Because of the poor reproducibility of this test method, it should be restricted to testing in only one laboratory when numerical abrasion resistance values are to be used. Interlaboratory agreement is improved significantly when rankings of coatings are used in place of numerical values. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels12 D 968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D 1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 D2240 Test Method for Rubber Property--Durometer Hardness3 4 3. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 Abrasion resistance can be expressed as one or more of the following terms: 3.1.1.1 wear index--1000 times the loss in weight in milligrams per cycle. 3.1.1.2 weight loss--the loss in weight in milligrams, 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.23 on Physical Properties of Applied Paint Films. Current edition approved May 25, 1990. Published July 1990. Originally published as D-4060 - 81. Last previous edition D 4060 - 84. 2 Annual Book ofASTM Standards, Voi 06.01. 3 Annual Book ofASTM Standards. Vol 09.01. determined at a specified number of cycles. 3.1.3 wear cycles per mil--the number of cycles of abra sion required to wear a film through to the substrate per mil of film thickness. 4. Summary of Test Method 4.1 The organic coating is applied at uniform thickness to a plane, rigid panel and, after curing, the surface is abraded by rotating the panel under weighted abrasive wheels. 4.2 Abrasion resistance is calculated as loss in weight at a specified number of abrasion cycles, as loss in weight per cycle, or as number of cycles required to remove a unit amount of coating thickness. 5. Significance and Use 5.1 Coating on substrates can be damaged by abrasion during manufacturing and service. This test method has been useful in evaluating the abrasion resistance of attached coatings. Ratings produced by this test method have corre lated well with ratings produced by the falling abrasive values in Test Method D 968. 6. Apparatus 6.1 Taber AbraserT 6.2 Abrasive Wheels--Resilient calibrase wheels No. CS- 10 or CS-17, as required, shall be used. Because of the slow ; ` hardening of the rubber bonding material in this type of wheel, the wheels should not be used after the date marked on them, or one year after their purchase if the wheels are not dated. N' 1--The hardness of the wheels can be cheeked by Test Method , D 2240. An acceptable hardness for both types of wheels is SI 5 units on Shore Durometer A-2 Scale. N' 2--The CS-17 wheels produce a harsher abrasion than the CS-10 wheels. 6.3 Resurfacing Medium, an S-ll abrasive disk, used lor resurfacing the abrasion wheels. 6.4 Vacuum Pick-Up Assembly, consisting of a vacuum unit, a variable transformer suction regulator, a nozzle with bracket attachment, and a connecting hose with adaptor. 7. Test Specimens 7.1 Apply a uniform coating ofthe material to be tested to a plane, rigid panel. Specimens shall be a disk 4 in. (100 mnn in diameter or a plate 4-in. (100-mm) square with rounded corners and with a 'A-in. (6.3-mm) hole centrally located on 4 Available from Teledyne Taber, North Tonawanda, NY 14120. 644 DU P050297826 A O 4060 _ JjL'h panel. Prepare a minimum of two coated panels for the ^ii.iterial. ' 3--The coatings should be applied in accordance with Test ytihods D 823, or as agreed upon between the purchaser and the seller. o t u 4--The thickness of the dry coatings should be measured in i'Ta rdance with Test Methods D 1005, D 1186, or D 1400. fr:: . pH. Standardization gig, 1 Mount the selected abrasive wheels on their respective `flange holders, taking care not to handle them by their " febrasive surfaces. Adjust the load on the wheels to 1000 g. -8 1 Mount the resurfacing medium (S-ll abrasive disk) 1ibra- mi] jj the turntable. Lower the abrading heads carefully until - wheels rest squarely on the abrasive disk. Place the fium pick-up nozzle in position and adjust it to a ance of l/32 in. (1 mm) above the abrasive disk. ;3 Set the counter to "zero" and set the suction regulator lsto idcd tpproximately 50 points on the dial. The setting may be leased to 90 if more effective removal of the abradings (fears necessary. 4 Start the vacuum pick-up and then the turntable of at a tder. Resurface the wheels by running them 50 cycles per unit inst the resurfacing medium. ' 5--The wheels should he resurfaced in this manner before ttg each specimen and after every 500 cycles. ton win bed 1 ` irelues Conditioning |l Cure the coated panel under conditions of humidity temperature as agreed upon between purchaser and JUnless otherwise agreed upon between purchaser and :r, condition the coated panel for at least 24 h at 23 2C !|50 5% relative humidity. Conduct the test in the same ronment or immediately on removal therefrom. SfProcedure |,1 Weigh the test specimen to the nearest 0.1 mg and fj$d this weight, if either the wear index or the weight loss > be reported. 1.2 Measure the coating thickness of the test specimen in eral locations along the path to be abraded. Ip Mount the test specimen on the turntable. Place the ^ailing heads on the test film and the vacuum pick-up lie in position as outlined in 8.2. Set the counter and Son regulator as outlined in 8.3. Ip Start the vacuum pick-up and then the turntable of jpbrader. Subject the test specimen to abrasion for the Sified number of cycles or until wear through of-the aiftig is observed. In determining the point of wear jgjtigh, stop the instrument at intervals for examination of fitest specimen. 10.5 Remove any loose abradings remaining on the test specimen by light brushing. Reweigh the test specimen. 10.6 Repeat 10.1 to 10.5 on at least one additional test specimen of the material under test. ,, 11. Calculation 11.1 Wear Index--Compute the wear index, /, of a test specimen as follows: / = (A - B) 1000 where: A = weight of test specimen before abrasion, mg, B = weight of test specimen after abrasion, mg, and C = number of cycles of abrasion recorded. N' 6--In calculating wear index it may be advisable to discard the last 200 cycles because the results may be affected by abrasion of the exposed substrate. 11.2 Weight Loss--Compute weight loss, L, of the test specimen as follows: L=A --B where: A = weight of test specimen before abrasion, mg, and B = weight of test specimen after abrasion, mg. 11.3 Wear Cycles Per Mil--Compute the wear cycles per mil, W, of the test specimen as follows: W -- D/T where: D -- number of cycles of abrasion required to wear coating through to substrate and T = thickness of coating, mils (0.001 in.) (to one decimal place). N' 7--In calculating the wear cycles, it is advisable to discard the first and last readings because the first may he affected by an uneven surface and the last by abrasion of parts of the substrate. 12. Report 12.1 Report the following information for each test mate rial: 12.1.1 Temperature and humidity during conditioning and at the time of testing, 12.1.2 Thickness of coating when wear cycles are speci fied, 12.1.3 Kind of calibrase abrasive wheels used, 12.1.4 Load applied to the abrasive wheels, 12.1.5 Number of wear cycles recorded for each test specimen, HI |~ Weight loss at 500 cycles Weight loss at 1000 cycles m>` Wear Index at 500 cycles |f;: Wear index at 1000 cycles || Cycles per mil TABLE 1 Precision of Taber Abrasion Values Within Laboratory Coefficient of Variation, % Maximum Allowable Difference, % 12 48 10 46 13 52 10 46 13 44 Between Laboratories Coefficient of Variation, % Maximum Allowable Difference, % 36 105 30 90 36 106 30 92 31 92 645 DUP050297827 ->v 0 4060 12.1.6 Wear index, weight loss, or wear cycles per mil for each test specimen, and 12.1.7 Mean and range of the abrasion resistance values of the replicate coated panels. 13. Precision5 13.1 On the basis of an interlaboratory test of this test method in which operators in five laboratories tested four coatings having a broad range of abrasion resistance, the within-Iaboratory coefficients of variation and betweenlaboratories coefficients of variation were found to be those in Table 1. Based upon these coefficients, the following s Supporting data are available from ASTM Headquarters. Request RR: D01-1037. criteria should be used for judging the acceptability of results at the 95 % confidence level: 13.1.1 Repeatability--Two results by the same operator should be considered suspect if they differ by more than the maximum allowable difference values shown in Table 1. 13.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than the maximum allowable difference values shown in Table 1. N' 8--When this test method is used to rank a series of coatings by magnitude of abrasion resistance, the precision is significantly better than shown in Table 1. In the interlaboratory study for evaluating precision, ail laboratories ranked the coatings in the same order of abrasion resistance. 14. Keywords 14.1 wear index The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination oI the validity of any such patent rights, end the risk of Infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, eitherreapproved or withdrawn. Your comments are invited either for revision ot this standard or for additionalstandards and should ba addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ofthB responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, PA 19103. 1 h t-- iiii 646 DUP050297828 Designation: D 4062 - 88 Standard test Method for Leveling of Paints by Draw-Down Method1 This standard is issued under the fixed designation D 4062; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last rcapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. his test method2 covers the laboratory determination relative leveling of water and solvent-reducible archi'jttU'al paints in white and light tints by comparing the Ills produced in a draw-down film to a series of plastic iding standards. ! Unpigmented, texture, and deep-tint coatings cannot ijt`i cadily evaluated with the shadowing produced by oblique jpjjng employed in this test method. Such coatings may be Kt by comparing them with the plastic standards at {Jjffius angles of reflection. For this purpose ordinary room jMjhg is satisfactory. bfjjs Since other factors may influence the tendency of "Sjttd paints to sag, this test method is not intended to ijlpure sagging. Bp This standard may involve hazardous materials, operJfljps, and equipment. This standard does not purport to Bfey all ofthe safety problems associated with its use. It is wjcWfsponsibility of the user of this standard to establish ' fmpriate safety and health practices and determine the I wbability ofregulatory limitations prior lo use. $?1: ! glpescription of Term Specific to This Standard "11: leveling--of a paint, a measure of its ability to flow , Jit,filer application so as to obliterate any surface irregularbites such as brush marks, orange peel, peaks, or craters, that jf-ijavcisbeen produced by the mechanical process of applica- ffiSiunimirv of Test Method m lij The material to be tested is presheared and then lapplied to a sealed chart by means of a special leveling test jBlljl designed to lay down a film with parallel ridges iJc'.iilating brush marks. After allowing the completed draw- jEdiro ii to dry in a horizontal position, leveling of the test paint gSated by viewing the draw-down under a strong, oblique ajgft source and comparing the contrast of lightness and pbw caused by the paint ridges to that of a series ofplastic png standards under the same lighting conditions. Significance and Use Instrumental evaluations of leveling by this test ' I'his lest method is under the jurisdiction of ASTM Committee D-l on Paint jljlllm Related Coatings and Materials and is. the direct responsibility of Subcom- j Ju** DO1.42 on Architectural Finishes. jUiirrent edition approved May 27, 1988. Published October j938. Originally ||ihed as D 4062 - 81. Last previous edition D4062 - 81 (1987). This lest method was essentially developed by the Leneta Company as PP^lUned in Leneta Catalog No. 3, pp. 26-7 (1976). method have been shown to correlate with those made by brush application. Leveling can affect the hiding and appear ance of applied architectural coatings, the presence of brushmarks and surface irregularities being more conspic uous with gloss and semi-gloss finishes than with flat finishes. 5. Apparatus 5.1 Leveling Test Blade3A--A grooved draw-down blade designed to lay down a wet film with parallel ridges (see Fig. D5.2 Draw-Down Plate, with two parallel, smooth-faced straightedges to guide the blade during film application and ensure that the ridges are straight 5.3 Syringe and Needle--A 10-mL LuerLok syringe and I'A-in. (38-mm) No. 15 gage needle for placing a fixed amount of the paint in front of the blade while simulta neously preshearing it (as during brushing) prior to drawingdown. Either glass or disposable plastic syringes may be used with water-reducible paints. Glass syringes only may be used with solvent-reducible paints due to swelling of disposable 'syringes by the solvent. 5.4 Test Chart*' plain white (for white or light tints) or predominantly black chart (for deep tints) coated with a suitable varnish or lacquer to render the test surface imper vious to the volatile portion of the paint. 5.5 Light Source37, 4o5bli*que, to illuminate the test draw down and leveling standards (see Fig. 2). 5.6 Levelness Standard^ -- Three-dimensional full-scale replicas ofdraw-downs made with the leveling test blade and nine paints exhibiting very poor to very good leveling, for comparison with the test draw-down. 5.7 Catch Papers, disposable, any type for catching excess paint is adequate. 3 The Leneta Leveling Test Blade, available from the Leneta Company. P. O. Box 86, Ho-Ho-Kus, NJ 07423, has been found satisfactory for this purpose. 4 The Leneta Leveling Test Blade used in this test method is a modification of the threaded draw-down bar described in an article by Dodge, J. S: "Quantitative Measures of Leveling," Journal of PahU Technology, Vol 44. No. 564, January 1972. 5 The Leneta Leveling Test Draw-Down Plate has been found satisfactory for this purpose. Available from the Leneta Company. A suitable draw-down plate may be constructed from the description given in 5.2 of this test method. * Leneta Form WB, a plain white sealed chart, and Leneta Form 7B, a biacJc and white sealed chart, available from the I-eneta Company, fjave been found suitable for light- and deep-tint paints, respectively. Equivalents may be used. 7 A standard oblique fluorescent light source (The Level-Luminator), has been found satisfactory for this purpose. Available from the Leneta Company. A suitable light source may be constructed from the description given in 6.5 and Fig. 2 of this test method. K Leneta Draw-Down Levelncss Standards, a series of nine 3 by 5 in. (75 by 125 mm) plastic full-scale replicas of draw-downs of paints having very poor to very good leveling, have been found satisfactory fot this purpose. Available from the Leneta Company. 647 DUPO 50297829 # D 4062 Stock is 130? stainless steel Dimensions: A--Length B--rDlameter C--1Supporting edge D--Minor doctoring edge 22 25 1.25 0.87 1.0 0.05 F--Minor clearance G--Clearance step H--Major clearance mm in. {ap prox.) 1.25 0.05 0.10 0.004 0.20 0.008 0.30 0.012 N' --This is actually a cylindrical rod. the term "blade" being employed as a conventional reference to film applicators. Auxiliary plastic side arms not shown. See Figs. 1 (b) and 1 (c). FIG. f (a) Leneta Leveling Test Draw-Down Blade 6. Preparation of Sample 6.1 Adjust the temperature of the paint to 73.5 3.5F {23 .2*C) or to a temperature agreed upon between buyer and seller. 6.2 Thoroughly mix the paint by hand with a spatula to a smooth, uniform composition and consistency to ensure that. the specimen to be taken for testing is representative. 7. Procedure 7.1 Affix the test chart to the draw-down plate. Position the leveling, blade at the far end of the chart, between the parallel straightedges, with, the longer arm of the blade adjacent to the left edge and pointing toward the ope^tor. 7.2 Place a catch paper just below but in contact wiffy the chart so that it is slightly to the right of the longer arm of the blade! 7.3 With the needle not attached, take up 8 to 10 mL of the material under test into the syringe (Note 1). Wipe offthe syringe orifice and attach the No. 15 gage needle. Eject within 3 to 5 s the entire amount in front of the blade forming a puddle. Immediately lay the syringe down, giasp the blade arms with both hands, and draw the leveling blade rapidly but smoothly over the test paint at a rate ofabout 2 ii (0.6 m) per s, keeping the long arm on the left parallel to the surface during the draw-down. N' 1--Filling the syringe arid cleaning the orifice are greatly facilitated by temporarily attaching to the orifioe a 2-in. (50-mm) length ofclear vinyl tubing with inside diameter of'/in. (3.2 mm) and outsider, diameter of Vis in. (5 mm), which is removed prior to attaching the, needle. 7.4 Allow the completed draw-down to dry overnight in .horizontal position, preferably at 73.5 3.5F (23 2C), and 50 5 % relative humidity, or under other conditium IS ; iifjta N' --Plastic sidearms are for guidance to assure rectiRnearity of blade movements. FIG. 1 (6) Photograph of the Leneta Leveling Test Draw-Down Blade N' --Illustration of use of draw-down plats and catch papers. Note tha* sidearms are attached to the test blade and parallel straightedge guides oh draw-down plate. FIG. 1 (c) Application With the Leneta Leveling Test Draw-Down Blade 648 DU P050297830 n 4062 teed upon between the buyer and the seller. 8. Report ,-'7.5 Place the dry draw-down, with its ridges perpendicular :'.fo the direction of the light, in front of the oblique light as *iown in Fig. 2. Place two leveling standards similarly nenlcd on either side of the test draw-down and view the 8.1 Report the leveling ofthe test paint on the scale of 0 to 10 as determined by comparison with the numbered leveling standards. ter portion of the draw-down and the standards from ive (that is at a 90" angle to the surface), or as close to 90" 9. Precision , possible if in a lighted room (see Fig. 2). Then successively 9.1 On the basis of a study in which seven operators, each j "interchange standards until one is found having the samuseing a different blade, rated twelve different paints, the ' . ;_(i linctness of lightness and shadow as the test draw-down. between-Iaboratories standard deviation was found to be 1.5 1 .T^e'clmg poorer than Standard No. 1 is designated as 0 or Tljfery poor leveling. Leveling better than Standard No. 9 is units on the 0 to 10 scale. Based on this standard deviation, the following criteria should be used forjudging the accept ' designated as 10 which represents perfect leveling or no ability of results at the 95 % confidence level: ' 'perceptible ridges. Estimate and record the number of the f tjveling standard that corresponds to the leveling of the test Ifcdown. 9.1.1 Reproducibility--Two results, each one by operators in different laboratories, should be considered suspect if they differ by more than 1.5 scale units. The American Society (or Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard ere expressly advised that determination of the validity ot any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received 8 lair hearing you should make your views known to the ASTM Committee on Standards. 1916 Race St.. Philadelphia, PA 19103. 649 DUP050297831 Designation: D 4082 - 89 Standard Test Method for Effects of Gamma Radiation on Coatings for Use in Light-Water Nuclear Power Plants1 This standard is issued under the fixed designation D 4082; the number immediately following the -designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers a standard procedure for evaluating the lifetime radiation tolerance ofcoatings to be used in nuclear power plants. This test method is applicable to Coating Service Levels I and It 2. Referenced Documents 2.1 ASTM Standards: D 659 Method of Evaluating Degree of Chalking of Exte rior Paints2 D 660 Test Method for Evaluating Degree of Checking of Exterior Paints2 D 661 Test Method for Evaluating Degree of Cracking of Exterior Paints2 D714 Test Method for Evaluating Degree of Blistering of Paints2 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints2 2.2 ANSI Standard:1 N512 Protecting Coatings (Paints) for Nuclear Industry 3. Significance and Use 3.1 Variations can occur in surface preparation, applica tion, and curing of coating materials. They may affect the performance of a coating system exposed to radiation when considered in conjunction with applicable engineered safety requirements. This test method is designed to provide a uniform test to assess the suitability of coatings, used in nuclear power facilities, under continuous radiation expo sure for the projected 40-year lifetime of the facilities, including radiation during a DBA. Specific plant radiation exposure may exceed or be less than the amount specified in 6.2 of this standard. The gamma dose used may exceed the actual anticipated plant gamma dose in order to account for expected beta exposure as well. Coatings in Level II areas (outside primary containment) are expected to be exposed to lower accumulated radiation doses. 4. Preparation of Test Samples 4.1 Steel Panels--Panels shall be prepared in accordance with ANSI N512. 1 This test method is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities and is the direct responsibility of Subcommittee D33.02 on Service and Material Parameters. Current edition approved Feb. 24, 1989. Published April 1989. Originally published as D 4082 - 83. Last previous edition D 4082 - 83. 2 Annual Book of ASTM Standards, Vol 06.01. 3 Available from American National Standards Institute, 11 W. 42nd St, 13th Floor, New York, NY 10036. 4.2 Concrete Blocks--Blocks shall be prepared in accord ance with ANSI N512. 5. Sampling 5.1 Prepare and test specimens at least in duplicate, or as: otherwise specified by the owner. 6. Procedures 6.1 Irradiation Dose Rate: 6.1.1 Make the gamma energy field at the position of th( test specimen 1 x 106 rads/h, or greater. It shall be urn mm to within 10% from one position of the specimen to another, 6.1.2 Make provisions so that all areas receive the sair.; average exposure and dose, if the specimen is irradiated by a nonuniform source. 6.1.3 Determine the dose rate by a procedure, acceptable to the coating manufacturer or as otherwise specified by the owner. 6.2 Irradiation Accumulated Dose--Make the total accu mulated dose 1 X 109 rads, unless otherwise specified by the ' owner. 6.3 Radiation Source--Simulate conditions at a reactor' site, closest to the preferred type of gamma source, such as, but not limited to, a fuel assembly. 6.4 Test Environment: 6.4.1 Specimens may be in air or in water during exposui t to the gamma source, depending on the intended sem. * as prescribed by the owner. ' 6.4.2 Do not exceed a temperature of 140F (60C) im the specimen during irradiation, or as otherwise acceptable Kb the coating manufacturer or as specified by the owner. 7. " Examination and Reporting 7.1 Examine and evaluate specimens immediately after! irradiation for the following coating defects: 7.1.1 Chalking (Method D 659)--Report extent. 7.1.2 Checking (Test Method D 660)--Report extent. 7.1.3 Cracking (Test Method D 661)--Report extent. 7.1.4 'Blistering (Test Method D 714)--Report number and extent. 7.1.5 Flaking- (Test Method D 772)--Report extent. 7.1.6 Delamination--Report extent. 7.1.7 Peeling--Report extent. 7.1.8 Report any observation of unusual appearance or deterioration. 8. Acceptance Criteria 8.1 Checking, Cracking, Flaking, Delamination, Peeling, and Blistering--None permitted. 650 DUP050297832 D 4082 Documentation . 1 Document the following: ;U The procedures and conditions relating to the test ;imen preparation. 1.2 The type of radiation source and the test procedure environment. 1.3 Both the initial dose rate and the total accumulated ET' ratory that shall not be affiliated in any manner with the coatings manufacturer unless otherwise specified by the owneT. 10.2 The testing laboratory shall be responsible for the documentation and certification of all test results. 10.3 The testing laboratory shall be responsible for meeting the quality assurance requirements of the owner. 11. Precision and Accuracy l i. I The precision and accuracy of this test method is Villi- Testing Laboratory , ^ VI Testing shall be conducted by an independent labo- reflected in the precision and certified accuracy of the test instruments used. ; 'Sr il B 7he American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments.are invited either for revision of this standard or for additional standards end should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you fee/ that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St. Philadelphia, PA 19103. 651 DU P050297833 Designation: D 4121 - 82 (Reapproved 1987) Standard Practice for Photographic Documentation of Coating and Lining Failures and Defects1 This standard is issued under the fixed designation D 4121; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A. number in parentheses indicates the year oflast reapproval. A superscript epsilon (<} indicates'an editorial change since the last revision or reapproval. ir 4 < !$ 1. Scope 1.1 This practice covers the requirements for photographs and photographic equipment to be used to document coating and lining failures or defects. Photographs may also be used to establish acceptance criteria. 1.2 The practice represents only one method to provide consistent, comparable photographs. The important factors to consider when using any type of photographic equipment are also described. 2. Significance and Use 2.1 The proper documentation, through photographic methods, in standard size and color is required for accurate comparison of a wide variety ofcoating and lining failures or defects. An integral part ofthe study ofdefects and failures is the ability to compare by a standardized reproducible method present and past appearances of defect characteris tics and failure modes. The equipment should not be complicated or require any special skill to produce good definition and color. 3. Requirements for Photographs 3.1 Requirements are as follows: 3.1.1 Color slides in 2 by 2-in. (50 by 50-mm) cardboard mounts, suitable for projection in ail standard 2 by 2-in. slide projectors, 3.1.2 Prints in a minimum 3 by 3-in. (76 by 76-mm) size. Unless a larger scale is needed, the standard Vh by 3`/2-in, (89 by 89-mm) size should be used. Prints may be either color or black and white, although color usually provides the greatest information to those viewing the photographs, and 3.1.3 A scale of the area photographed. 4. Requirements for Standardized Photographic Equipment 4.1 The equipment should consist of the following:2 4.1.1 A 3 by 3-in. (76 by 76-mm) copy stand complete with compensating lense. The focal depth should be approx imately Vs in. (10 mm) above the subject plane to approxi mately `A in. (6 mm) below the subject plane. 4.1.2 An 8 by 8-in. (203 by 203-mm) copy stand complete with compensating lense. The focal depth should be approx imately l`/2 in. (38 mm) above the subject plane to approx imately 1 in. (25 mm) below the subject plane. 1 This practice is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.Q3 on Quality Systems. Current edition approved March 26, 1982. Published May 1982. 1 The Kodak Ektagraphic EF Visualmaker satisfies the requirements of this practice. 4.1.3 A camera that will accept 12 or 20 exposures 1 'i size cartridge and have a lens system compatible with tlx copy stands in accordance with 4.1.1 and 4.1.2. 4.1.4 A flash cube or an electronic flash unit designe, specifically for use with the camera-stand assembly. Tlx electronic flash should have approximately a 40-s recovery time. The electronic flash should be battery-operated and sell contained.. 4.2 Equipment other than that described above may be used for photographic documentation; but, there may be varying scales and lighting effects. 5. Precautions and Limits 5.1 The following factors are the principal variables af fecting photograph clarity over which the user has control 5.1.1 Degree ofEnlargement--Enlarging a given negative beyond a certain point yields no additional clarity to the photographs; more clarity must come from either a larger or clearer negative. Enlargement should be great enough so sufficient detail can be seen without the use of a magnifying glass. 5.1.2 Negative Size--The larger the negative, the more detail and clarity it can record. It is suggested that . minimum negative size of 26 by 26 mm be used. Negati . sizes much larger that this might be needed rarely, if ev ' 5.1.3 Film Speed--"Faster" films have progressively less resolution. In general, 35-ttim ASA 200 film gives poor resolution ifenlarged much beyond 4 by 5 in. when printiu 5.1.4 Lighting--Insufficient lighting gives poor resolu tion. Lighting of the wrong color such as incandescent bulbs using daylight film, distorts colors. Bright lights or fla-b perpendicular to a glossy or shiny surface causes glare. Also, perpendicular lighting may fail to show surface irregularities. Lighting at too oblique an angle may exaggerate the irregu larities. 5.1.5 Camera Stability--A rigid support such as a copy stand or tripod will minimize camera movement. 5.1.6 Camera Optics and Quality--Professional quality cameras and equipment may be impractical due to cost, difficulty ta operate, delicacy of equipment, or the need for an immediate print. Acceptable photographs can be obtained with some of the simpler, good-quality cameras. 6. Documentation 6.1 Each photograph shall be identified with the following information: 6.1.1 Date and time of photograph, 6.1.2 Where the photograph was taken and what it i* intended to show, and 6.1.3 Name of the photographer. 652 M DUP050297834  D 4121 The Amerlcen Society for Testing end Materials takes no position respecting the validity of anypatent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed Bvery five yews and if not revised, either reepproved or withdrawn. Yourcomments are Invited either forrevision of this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive carefiii cons/tferatfon at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 653 DUP050297835 Designation: D 4138 - 88 Standard Test Method lor Measurement of Dry Film Thickness of Protective Coating Systems by Destructive Means1 This standard is issued under the fixed designation D4I38; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A numherin parentheses indicates the year oflast reapproval. A superscript epsilon <t) indicates an editorial change since the last revision or rcapproval. 1. Scope 1.1 This test method covers the measurement of dry film thickness of coating films by microscopical observation of precision-cut angular grooves in the coating film. Field use of this method may require repair of the coating film. 1.2 The substrate may be any rigid material, for example, metal, plastic, concrete, glass, etc. The surface may be plane or moderately curved (pipes as small as 1 in. (25 mm) in diameter may be measured in the axial direction). 1.3 This test method is not recommended for excessively elastomeric or excessively brittle films, although cooling or heating the surface can often modify the coating in the desired direction. 1.4 The range of thickness measurement is 0 to 50 mils (0 to 1.3 mm). 1.5 Measurements may be made on field structures, on manufactured products, or on test panels. 1.6 This standard may involve hazardous maierials,-operalions, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safely and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 3. Significance and Use 3.1 Measurement ofdry film thickness of organic coatings by physically cutting through the film and optically ob serving and measuring the thickness offers the advantage of direct measurement as compared with nondestructive means. 3.2 The use of this test method is not necessarily limited by the type of substrate material as are nondestructive magnetic-type means. 1 This test method is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities. Current edition approved Feb. 2d, 1988. Published April 1988. Originally published as D4I38 -82. Last previous edition D 4138 - 82. 2 Annual Book ofASTM Standards, VoJ 06.01. 3.3 Constituent coats of an overall thickness of a coatmg system can be measured individually by this method. 4. Apparatus 4.1 The measurement shall be performed by first incising a scribe mark of known configuration through the coating(s) film to substrate and then viewing the scribe mark with an illuminated microscope with measuring reticle. Scribe cutter' and illuminated microscope may be combined as a single instrument (see Fig. I).3 Instrument calibration shall be performed by taking measurements on applied filtm i-f known thickness. (See Test Methods D 1005.) 4.2 The configuration of the tungsten carbide cutting tips shall be designed to provide a very smooth incision in the paint film at a precise angle to the surface (see Fig. 2). Separate tip designs (angles) shall provide cuts of known slopes such as 1 to 1, 1 to 2, and 1 to 10. These tips shall bn nominally designated lx, 2x, and lOx to indicate the r.ii-.j of the lateral measurement (microscope) to film thickness-' (cut depth in film). Metal guide studs on the gage body shall, together with the cutting tip, form a firm base to assure that the tip aligns vertically with the painted surface for precisely aligned incision. 4.3 The illuminated, 50-power microscope shall contain alj reticle scaled from 0 to 100 divisions (see Fig. 3). The total1!*2 viewing field of the microscope shall be approximately IT" mils (3.18 mm). 5. Test Specimens 5.1 If multiple coats of paint are to be measured, sur sive contiguous coats should be of contrasting colors to aidS sharp discrimination of interfaces. 5.2 Generally, test specimens shall be prepared (as test! panels) or chosen (as sites on a structure) to be represent,T r. G . of localized coating thickness and variability. 'if 5.3 For test panels, if measurement repeatability is desiredj for a particular paint system, painstaking care shall be taken; in panel preparation. Steel panels shall be ground plane or* rolled to 8.5-p.in. (215-nm) inches flatness. Coating shall be' uniformly applied in accordance with Test Methods D 823. Panels shall be placed in a horizontal position during drying. ` Uniform application thickness shall be verified by another) measurement method such as Test Methods D 1005. 6. Procedure 6.1 Select a test panel or choose a site for thickness measurement. 'A Tooke Gage, manufactured by Micrometries, P.O. Box 13804, Atlanta, GA 30324, has been found suitable for this purpose. 654 DUP050297836 # D 4138 aim;> hit FIG. 1 Tooke Inspector Gage--Model Mark II | Using an appropriate surface marker of contrasting i!j mark a line on the surface about* 2 in. long. 13 Select a cutting tip based on estimated film thickness follows: Thickness Range, mils (mm) Conversion Factor 20 to 30(0.51 to 1.3) 1.0 2 to 20 (0.05 to 0.51) Oto 3(0 to 0.76) 0.5 0.1 ^thickness is unknown, make a trial determination with Vx tip. f To incise a groove, grasp the gage with the studs and ting tip firmly forming a tripod on the painted surface. c| the gage at right angles to and about 2 in. (51 mm) endicularly from a marked line. 6.5 Draw the gage across .the paint film toward the body, with guide studs leading the cutting tip, and increase pressure on thecutrihg tip until it barely cuts into the substrate before it crosses the marked line. 6.6 Take readings at the intersection of the marked line and incision. Read by measuring on the reticle the distance from the substrate/coating demarcation up the longer ma chined slope of the incision to the upper cut edge of each respective coating or the coating system. Make sure that the machined dope of the incision is measured, not the other, steeper slope. (The machined upper edge usually leaves a less jagged cut than the other side.) Ifmultiple coats are observed, individual thicknesses of each coat may be read The actual coating thickness is derived by multiplying the reticle reading by the conversion factor for the respective cutting tip. FIG. 2 A' A FINISH COAT THICKNESS B' - B - PRIMER COAT THICKNESS Typical Incision Provided by Tungsten Carbide Cutting Tip of Tooke inspector Gage 655 ail DUP050297837 # D 4138 7, Report 7.1 Report the following information: 7.1.1 Results ofa Thickness Determination--If more than one measurement is made and specific results for each location are not needed, report the minimum, the max imum, and the average thickness. 8. Precision 8.1 The replicability of individual observations of a uni form coating on a smooth substrate has been determined to be within --10 %. (The percentage error increases as film thickness decreases.) 8.2 Field-applied coatings are characteristically subject to short-range thickness variability resulting from rough sub strates and erratic application. The magnitude of this vari ability will be sensitively reflected by the range or standard deviation of thickness determinations. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsive technical committee and must be reviewed every five years and If not revised, either reapproved or v/Hhdrawn. Your comments ere Invlteld either torrevision of this standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful conslderet/on at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. > DU P0502 97838 ft Designation: D 4141 - 82 (Reapproved 1987)e1 jmifej;-. Standard Practice for Conducting Accelerated Outdoor Exposure Tests of Coatings1 This standard is issued under the fixed designation D414I; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates aii editorial change since the last revision or reapproval. N' --Footnote 3 was editorially changed in November 1987. jpppe jjf'This practice covers three accelerated outdoor expoprocedures for evaluating the exterior durability of ings applied to metal substrates. The three procedures are as follows: ;;i Procedure A--Black Box Exposure. |i2' Procedure B--Heated Black Box Exposure. .3 Procedure C--Fresnel Reflector Rack Exposure. jJiThe durability rankings of coatings provided by these procedures may not agree when coatings differing y in composition are compared. ("The acceleration of degradation rates of coatings ^*/^jUced by the three procedures of exposure are discussed. t 1--Other exposure procedures may provide accelerated results types of products. ' SB This standard may,involve hazardous materials, operAnd equipment. This standard does not purport to JHpf all ofthe safety problems associated with its use. It is IfffiSipansibility of the user of this standard to establish mW^i'$.riate safety and health practices and determine, the Tgptffrjbilily. of regulatory limitations prior to use. WnRefcrenced Documents WmvASTM Standards: Test Method for Specular Gloss2 ` >59 Test Method for Evaluating Degree of Chalking of nInterior Paints2 .jjm'O Test Method for Evaluating Degree of Checking of "Imferior Paints2 31 Test Method for Evaluating Degree of Cracking of Jgpteriar Paints2 rapMl Test Method for Evaluating Degree of Blistering of Ijjfcnts2 P3 Test Methods for Producing Films of Uniform Bjfjhickness of Paint, Varnish, and Related Products on gist Panels2 `, P'86 Test Methods for Nondestructive Measurement of itty Film Thickness of Nonmagnetic Coatings Applied 11% Ferrous Base2 J244 Test Method for Calculation of Color Differences pom Instrumentally Measured Color Coordinates2 E 838 Practice for Performing Accelerated Outdoor Weathering Using Concentrated Natural Sunlight3 G7 Practice for Atmospheric Environmental Exposure Testing of Nonmetallic Materials4 3. Summary of Practice 3.1 Several procedures that will provide accelerated rates for the degradation ofcoatings are descri&ed. The procedures appear in the following order: 3.1.1 Procedure A--Exposure on a black box panel rack facing the equator at 5 from horizontal. 3.1.2 Procedure B--Exposure on a heated black box panel rack facing the equator at 5" from horizontal. 3.1.3 Procedure C--Exposure on a Fresnel reflector panel rack that provides a high intensity of sunlight irradiation by following the sun and focusing the sunlight on the test panels ,t>y means of mirrors. The panels are wet periodically by deionized water spray.5 3.2 Each of these procedures requires that coated test panels be placed on racks of specified design and be exposed under specified conditions of weathering. 3.3 The selection of a procedure for producing accelerated degradation is. dependent on the intended end use of the coatings, limitations on the time available for the exposure tests, and the degree of reliability required for predictions of durability performance. 4. Significance and Use 4.1 The procedures described in this practice are designed to provide greater degradation rates of coatings than those provided by fixed angle outdoor exposure racks that opti mize the annual incident solar radiation. For many products, fixed-angle exposures accelerate the normal end-use rate. , 4.2 Following are comments regarding the relative rates of degradation that can be expected for coatings exposed by the procedures described in this practice. 4.2.1 Procedure A (Black Box)--For many coatings, this procedure provides greater rates of degradation than those provided by 5, equator-facing, open-rack exposures because the black box produces higher panel temperatures during irradiation by the sun and longer time of wetness. The black box panel temperatures are comparable to those encountered jrJvMS practice is under the jurisdiction of ASTM Committee D-l on Paint and Coalings and Materials and is the direct responsibility of Subcommittee on Accelerated TesLS for Protective Coalings, rent edition approved June 25, 1982. Published Augtist 1982. bitted Book ofASTM Standards, Vof 06.01. 3 Annua! Book ofASTM Standards, Vols 12.02. 4 Annual Book ofASTM Standards, Vol 14.02. 5 Fresnel reflector panel racks arc located at DSET Laboratories. Inc., Box 1850, Black Canyon Stage 1, Phoenix, AZ 85029 and South Florida Testing Service Inc., Desert Site, 31818 N. 203rd Ave., Whittman, AZ 85361. 657 DUP050297839 D 4141 on the hoods, roofs, and deck lids of automobiles parked in direct sunlight. 4.2.2 Procedure B (Heated Black Box)--This procedure is most useful for exposures conducted in the late fall, winter, and early spring when it produces significantly higher panel temperatures than those produced by the 5", equator facing, black box. Therefore, thisprocedure produces greater rates of degradation than those produced by Procedure A, particu larly in the case of coatings with rates of degradation that are very temperature dependent. N' 2--The relative rates of gloss loss and color change produced in some automotive and coil coatings by exposures in accordance with Procedures A and B are given in ASTM Special Technical Publication 781.6 4.2.3 Procedure C (Fresnel Reflector Rack)--This method provides greater rates of degradation of coatings than those provided by Procedure A or Procedure B. This high acceler ation is produced by very high sunlight intensity and high panel temperature. 4.2.4 THe degradation rates produced by any of the three procedures depend on the seasons of exposure, geographical location, and type of coating. The rates are higher in late spring, summer, and early fall when the intensity of sunlight irradiation is the greatest and when panel temperatures are higher. Also, the rates are highest for exposures in warm, humid environments. '' 4.2.5 Because outdoor weather conditions vary from season to season and year to year, these procedures are not reliable for establishing absolute performance ratings for coatings. The procedures should be used only for comparing the relative performance of coatings exposed at the same time at the same location. 5. Test Specimens 5.1 Each test specimen and control specimen shall, consist of a uniform coating applied to the surface of a rigid panel. Suitable application procedures are given in Test Methods D 823. 5.2 Use surfaces of good planarity because warpage, waviness, or curvature may seriously affect the measure ments of gloss and color and may produce a poor air seal on the black box rack. 5.3 Control specimens shall be prepared for inclusion in each exposure series to act as comparison standards and to provide a means for determining the severity ofthe exposure conditions encountered by the series. For best results, there should be at least two controls differing significantly in their durability performance. 5.4 Using Test Methods D 1186, measure the dry film thickness of the coatings at several different positions on the test and control specimens. PROCEDURE A--BLACK BOX EXPOSURE 6. Apparatus 6.1 Black Box Rack of materials and construction as described in Practice G 7, or its equivalent. Symposium on Pcrformanence of Organic Coalings. ASTM STP 78/, ASTM, 1982. 7. Procedure 7.1 Position the rack so that the surfaces of the test specimens are 5 from the horizontal, facing the equator. 7.2 If change in gloss is to be measured, determine the specular gloss value for each unexposed specimen using a properly calibrated glossmeter in accordance with Test Method D 523. 7.3 If change in color is to be measured, determine the color coordinates for each unexposed specimen using Method D 2244. Unless otherwise agreed upon, use the C1E Lab Instrument Color Scale. The color-measuring instru ment shall be stable and properly calibrated. N' J--As an alternative procedure, reserve unexposed duplicate specimen panels of each coating as reference for color difference measurements to be made on the exposed specimens. To minimize color drift, store these panels in a refrigerator. 7.4 Mount and fasten the specimens on the exposure rack, i All empty spaces on the rack should be covered by dark gray or black panels so that the entire surface of the rack is;; covered. N' 4---The predominant color of the specimen panels on the black box as well as the temperature of a standard panel should be noted. A panel on a black box will attain a lower temperature if all the other panels are white than ifall the other samples are black. 7.5 Expose the test and control specimens for a specified period of time on the basis of one of the following: j 7.5.1 Exposure for a specified number ofdays, months,orl years with respect to an agreed upon starting date, j 7.5.2 Exposure to a specified quantity of irradiation, !| 7.5.3 Exposure until a specified physical change hi-j occurred in the test specimens, or | 7.5.4 Exposure until a specified change has occurred in a j control specimen exposed with the test specimens. 7.6 Remove the specimens from the exposure rack and j gently wash a portion of the specimen surfaces to removes loose dirt. A suitable procedure consists of gentle rubbing) with a sponge wet with .water or a 0.05 % solution of n) nonionic detergent. Water droplets should be gently remoi u! j from the specimen surfaces to prevent water spotting. 7.7 Unless otherwise agreed upon, perform the following; on the washed portion of each washed specimen: 7.7.1 Measure the specular gloss by Test Method D 523. j 7.7.2 Measure the color coordinates by Method D 2244,j using the same color scales as used for measuring lliej unexposed specimen. j 7.7.3 Checking rating by Test Method D 660. ; 7.7.4 Cracking rating by Test Method D 661. " 7.7.5 Blistering rating by Test Method D 714. j 7.8 Unless otherwise agreed upon, perform a chalk ratin';; by Method D 659 on an unwashed area of the specimen. PROCEDURE B--HEATED BLACK BOX EXPOSURE 8. Apparatus 8.1 Black Box Rack of materials and construction as described in Practice G 7, or its equivalent. The rack shall be equipped with a device that can heat the air in the interim ot the box to the specified temperature. 8.2 Safety Precautions--The heated black box rack must be properly grounded to prevent possible electrical shoe'-. 658 DUP050297840 ft D 4141 jge heating elements in the heated black box must be . so that, in normal use, a person cannot come in " ippontact with a hot surface. Procedure **! 9-1 Position the rack so that the surfaces.of the test ne t,e using eClE nstru- eeimens are 5" from the horizontal, facing the equator. K9 l If change in gloss is to be measured, determine the *j-.spLcalar gloss value for each unexposed specimen using a properly calibrated gloss-meter in accordance with Test jjlKlethod D 523. "s^r 9.3 If change in color is to be measured, use the procedure '7-wK`ii in 7.3. 1 B' K9,4 Mount and fasten the specimens on the exposure rack. <SAH mpty spaces on the rack shall be covered by dark gray or jifeack panels so that the entire surface of the rack is covered. ` " Set the air temperature controller inside the heated l|k box to maintain an air temperature of approximately [JSF (60C) or other agreed upon temperature. J|.6 The heater shall be turned on at approximately 9 a.m. ; |||; day and turned off at approximately 3 p.m. each day. R7 Expose the specimens for a specified period on the ipis of one of the procedures outlined in 7.5.1 to 7.5.4. |8 Remove the specimens from the exposure rack and HlBy wash a portion of the specimen surfaces to remove ; dirt. Use the procedure recommended in 7.6. |9 Unless otherwise agreed upon, perform the following >||he washed portion of each specimen: j}9.1 Measure specular gloss by Test Method D 523. jj9.2 Measure the color coordinates by Method D 2244, ; the same color scales as used for measurements of the exposed specimen. (19.3 Checking rating by Test Method D 660. 9.4 Cracking rating by Test Method D 661. jl$9.5. Blistering rating by Test Method D 714. Kps IO Unless otherwise agreed upon, perform chalk rating Slethod D 659 on an unwashed portion of the specimen. PROCEDURE C- FRESNEL REFLECTOR RACK EXPOSURE . apparatus |,0.1 Fresnel Reflector Exposure Rack that follows the [ concentrates sunlight irradiation on the test specimens IJneans of mirrors, and sprays deionized water on the feces of the test specimens at specified intervals. The rack a[f have provisions for cooling the test specimens while fuv are irradiated. Refer to Practice E838 for detailed riptions of the apparatus. ng ). [Procedure . 1 If change in gloss is to be measured, determine the cular gloss value for each unexposed specimen. The i-meter used shall be properly calibrated. J.11.2 If change in color is to be measured, use the Ebcedure given in 7.3. 11.3 Mount and fasten the specimens on the exposure rack. 11.4 Set the water spray control to provide a deionized water spray on the specimens during tlie'night at a frequency of 4 per hour, each spray period to. be of 3-min duration. Refer to Procedure B of Practice E 838 for detailed operating procedures. 11.5 Expose the specimens for a specified period on the basis of one of the procedures outlined in 7.5.1 to 7.5.4. 11.6 Remove the specimens from the exposure rack and gently wash a portion of the specimen surfaces to remove loose dirt. Use the procedure recommended in 7.6. 11.7 Unless otherwise agreed upon, perform the following on the washed portion of each specimen: 11.7.1 Measure specular gloss by Test Method D 523. 11.7.2 Measure the color coordinates by Method D 2244, using the same color scales as used for measurements of the unexposed specimen. 11.7.3 Checking rating by Test Method D 660. 11.7.4 Cracking rating by Test Method D 661. 11.7.5 Blistering rating by Test Method D 714. 11.8 Unless otherwise agreed upon, perform a chalk rating by Method D659 on an unwashed portion of the specimen. 12. Evaluation of Results 12.1 Express the change in gloss of each specimen either in terms of units of gloss loss or in percent gloss loss relative to the initial gloss value. 12.2 Express the change in color of each specimen in terms of total color difference, AE, using one of the procedures given in Method D 2244. 12.3 Express the amounts of chalking, checking and cracking on a scale of 10 to 0 as outlined in Method D 659, Test Method D 660 and Test Method D 661, respectively. 13. Report 13.1 Report the following information: 13.1.1 The method of exposure used and its geographical location. 13.1.2 The duration of the exposure and the date of the beginning of the test. 13.1.3 The heated black box air temperature used (for Procedure B). 13.1.4 The type of control specimens used and the se verity of their degradation. 13.1.5 The evaluation measurements performed on each of the exposed specimens: 13.1.5.1 Units of gloss loss or percent gloss loss. 13.1.5.2 Units of AE color change. Denote the color space and color scales used. 13.1.5.3 Ratings for chalking, checking, cracking, and blistering. 659 DUP0502 97841 D 4141 The American Society for Testing and Materials takes no position respecting the validity of any patent rights assertedin connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, ere entirely their own responsibility. This standard Is subject to revision al any time by the responsible technical committee and must be reviewed every five years and if not revised, either reepproved or withdrawn. Yourcomments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive cerelul consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia. PA 19103. 660 DUP0502 97842 Designation: D 4144 - 82 {Reapproved 1987) V Standard Method for 4/.1' Estimating Package Stability of Coatings for Ultraviolet m, Curing1 tv This standard is issued under the fixed designation D4144; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A. number in parentheses indicat the year oflast reapproval. A J superscript epsilon (0 indicates an editorial change since the revision or reapproval. mOf! t Scope 4.4 Spheres, glass or porcelain, 7 to 10-mm diameter. "jtH This method covers procedures for testing the package g|ity of coatings intended to be cured by ultraviolet S|ion. One procedure is given for clear coatings and er for opaque fillers. (E This standard may involve hazardous materials, opergjj, and equipment. This standard does not purport to ;ss all ofthe safety problems associated with its Use. It is Wksponsibility of the user of this standard to establish Wpriate safety and health practices and determine the mobility ofregulatory limitations prior to use. g||mmary of Method ijiiSpecimens are placed in several containers, some of ^are subjected to an elevated temperature while others jflpred at room temperature. At specified intervals a Tljen is checked for evidence of gelling. Clear materials Sid in glass containers so they can be examined visually npt opening to prevent contact with air which might pi polymerization. Opaque materials are checked by ||g one can, probing the contents with a spatula to ne the extent of any polymerization, and then "Jprng that specimen. Significance and Use Coatings intended to be cured by ultraviolet radiation, pDy those involving free radical chemistry, tend to 1%Wze during storage. It is ofinterest to determine how j|| fonnulation resists this effect. Many factors influence ~ storage stability of a composition. The procedures Jfed here are intended to improve the precision of lining this property. Because the effects of resins, 3g|ners, photoinitiators, synergists, stabilizers, or pigM can alter the relation between elevated and room gpature stabilities, any correlation of performance at Afferent temperatures is possible only with a given Jjlhtion and, therefore, is useful only for quality control. (paratus Oven, maintained at 60 2C. fClass Jars, wide-mouth, 4-oz (115-mL), with 38-mm 5jes. Cans, lined, 4-oz (115-mL), friction top, with lids. phis method is under thejurisdiction of ASTM Committee !>I on Paint and hd Coatings and Materials and is the direct responsibility of Subcommittee *c2 t n Factory-Coated Wood Products. "'em edition approved June 25, t982. Published September 1982. 5. Procedure 5.1 Clear Coatings: 5.1.1 Fill three 4-oz (115-mL) wide-mouth jars to Vain. {6 mm) from the top. Add a small glass or porcelain sphere to each container and put the lids on tightly. 5.1.1.1 The amount ofhead space in ajar or can is critical because the volume of air in contact with the sample has an effect on the rate of polymerization. The stability is also related to the ratio of the area of liquid-air interface to the volume of liquid. 5.1.2 Put twojars in an oven at 60 2C. Retain the third at ambient temperature, 25 2C, and in the dark. 5.1.3 Check an oven jar daily but do not open or invert. Rather, tip slightly, no more than 30, to determine the extent of polymerization by noting the mobility of the sphere. When gelling is noticed, check the second jar to confirm. 5.1.4 Record the duration of the test in days. Indicate the last day the sphere is mobile followed by the first day it is immobile, and if the days are not consecutive, why the interval occurred. 5.1.5 Check the jar stored at room temperature every week-but do not open or invert. Tip slightly, no more than 30, to determine if the sphere is immobile. 5.1.6 Record the number of weeks not gelled followed by the first week the sphere is immobile. 5.2 Pigmented (Opaque) Coatings: 5.2.1 Fill twelve 4-oz (115-mL) lined cans to lA in. (6 mm) from the top and put the lids on tightly. 5.2.1.1 See 5.1.1.1. 5.2.2 Put six of the cans in an oven at 60 2C. Retain six cans at ambient temperature, 25 2C. 5.2.3 After one day remove one can from the oven, open, and probe to the bottom to determine if gelling is beginning. Discard the can after the test. Check one of the remaining cans on the 2nd, 4th, 8th, 16th, and 32nd days and discard after testing. By starting on a Monday all the testing will fall on normal working days. 5.2.4 Record the condition of the specimen each day tested, indicating the fractional amount of any gelled mate rial present. 5.2.5 After one week check one of the cans held at ambient temperature by opening and probing to the bottom to determine ifgelling is beginning. Discard the can after the test. Check one ofthe remaining cans after 2,4,8,16, and 32 weeks. 661 DUP050297843 D 4144 5.2.6 Record the condition of the specimen after each test and indicate the fractional amount of any gelled material present. 6. Report 6.1 Report whether the material was clear or pigmented and the length of time it was stable as indicated by the occurrence of gelation at both ambient and elevated temper atures. Report the age of the material when the test began, if it is known. 7. Precision 7.1 Clear Coatings: 7.1.1 At the elevated temperature, four of five cooperators reported a clear coating without inhibitor gelled on the 8th or 9th day. Four of five cooperators reported a coating with inhibitor gelled on the 32nd day; the fifth reported gelation on the 18th day. 7.1.2 At room temperature four of four cooperators reported no gelling at 32 weeks, with or without inhibitor. 7.2 Pigmented Coatings: 7.2.1 At the elevated temperature six of six coopeiators reported a filler gelled at 8 days. 7.2.2 At room temperature four of four cooperators reported various degrees of gelation after 32 weeks. The American Society lor Testing and Materials takes no position respecting (lie validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement oi such rights, are entirely their own responsibility. This standard (s sub/ect to revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised,t either reapproved or withdrawn. Your comments are Invited either forrevision of this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 662 DUP050297844 Designation: D 4145 - 83 {Reapproved 1990)1 Standard Test Method for Coating Flexibility of Prepainted Sheet1 This standard is Issued under the fixed designation D 4145; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicales an editorial change since the last revision or reapproval. ei N' --Section 2 was deleted and editorial changes were made throughout in May J 990. 4 Scope ll This test method describes a procedure for deterliimg the flexibility and adhesion of organic coatings tints) on metallic substrates that are deformed by bending ,en the sheet is fabricated into building panels or other duets. E,2 The metal substrate must be capable of passing, this es[ without fracturing and with no excessive grain developItnt. : This standard does not purport to address the safety uhlans associated with its use. It is the responsibility ofthe of this standard to establish appropriate safety -and iuth practices and determine the applicability ofregulatory nions prior to use. BTenninology 1 Description of Term Specific to This Standard: fl I ' T-bend--a description of the severity of a bend in finis of the thickness (T) of the sheet to which the coating been applied; as used in this test method, the T-bend ng is the minimum number of thicknesses of metal li'nii d which the coated sheet is bent (Fig. 1); or if bent i id a die, the number of thicknesses ofmetal equivalent he diameter of the die to achieve no fracture or removal he coating. Summary of Test Method 3.1Prepainted panels are bent 180 around progressively re thicknesses of meial or larger diameter dies, the end ini being when failures no longer occur. The panels are 'jammed at low magnification (5 to lOx) after each'bend for ture of the coating (cracking) and, for loss of adhesion choff, by means of a tape pull-off test. Significance and Use p.l Organic coatings on precoated sheet are subjected to s,,<.s when fabricated into products by roll forming, brake fcpnJ'ng, or other deformation processes. These stresses can ed the flexibility or adhesive strength of the coating, suiting in fracture of the coating, exposing the substrate, or it adhesion to the substrate. This test is a means of Ifaluating the ability of a coating system to withstand the fcho'.st.s of fabrication. Tins test method is under the jurisdiction of ASTM Committee D-J on Paint Jd Related Coatings and Materials and is the direct responsibility of Subcom-Jpttcc DO 1.53 on Factory-Prccoated Strip Metal. liPCuTrem edition approved March 25, 1983. Published July 1983. 4.2 The bend direction, whether the axis of bend is across or along the rolling diameter of the metal, and the tempera ture of the specimen when it is bent affect the results of this test and should be agreed upon between the supplier and the user. 5. Apparatus 5.1 A means of holding one end of the specimen rigidly while making the bend is needed. A bench vise with smooth jaws or with smooth inserts, preferably of a soft metal to avoid damage to the coating, has been found to be satisfac tory. 5.2 If the metal is not bent around itself as in Fig. 1, a series of bending dies with smoothly rounded ends may be used as guides around which the specimen is bent (Fig. 2). 5.3 Magnifier, capable of 5 to lOx magnification for examining the specimen for coating fracture and pickoff after testing. A stereomicroscope has been found useful for this purpose. 6. Procedure 6.1' Bending the Coated Specimen Around Itself. 6.1.1 The coated specimen shall be at least 2 in. (50 mm) across the bend direction, by a length sufficient to make the required number of bends. A 2 by 6-in.'(50 by 150-mm) size is convenient. The specimen shall be at 2F of the temperature agreed on. N' --A triangle-shaped specimen (Fig. 3) has been found conven ient for making T-bend-tdsts. This shape leaves a portion of each bend exposed for later examination and for a permanent record. 6.1.2 Secure about 0.5 to 0.75 in. (13 to 20 mm) of one end of the specimen in a vise or holding jig as shown in Fig. 1. Bend the free end of the specimen 90 in a smooth and uniform manner so that the coating is on the outside of the specimen after it is bent. 6.1.3 Continue to bend the specimen until the bent end can be inserted in the jaws of the vise. Tighten the vise to complete the 180 bend, which is called an OT bend. Take care to tighten the vise sufficiently so that the apex of the bend is as flat as can be reasonably achieved. 6.1.4 Examine the bend using a hand lens or low-power microscope for cracks in the coating. 6.1.5 Apply pressure-sensitive tape2 along the bend. Rub the tape flat; then, holding the specimen firmly, remove the 2 Scotch Brand #610 tape manufactured by 3M Co., St. Paul, MN or equivalent, or as agreed upon between the supplier and the user. 663 DU P050297845 IWSERT THIS END N VISE--< . !-TeS" D 4145 COATED SURFACE N' --The above bends are expanded for clarity. They are actually flat against themselves In the^tesf. FIG. 1 T-Bend Test in Which the Coated Specimen ip Bent. Around Itself tape with a rapid.movement at an angle of 180" to the bend surface. Examine the tape for coating removed from the surface of the specimen (that is, pickoffiji. In the case of a coated steel specimen (for example, galvanized steel), ex amine the tape to determine whether pickoff is between the organic coating and the metallic surface or between the metallic coating and the base steel. 6.1.6 Secure the bent end of the specimen in the vise and bend the free end 90. Continue to bend the free end around the first (OT) bend to complete a 180 bend, and tighten in the vise as before. This makes a IT bend (Fig. 1). Examine under magnification and by taping for cracking and pickoff, as with the OT bend, 6.1.7 Repeat this procedure, making a 2T, 3T, etc., bends until no cracking or pickoff occurs. 6.2 Bending the Coated Specimen Around a Die: 6.2.1 The coated specimen shall be at least 2 in. (50 mm) across the,bend direction. ` N' --The above bends are expanded lor clarity. They are actually flat against themselves in the test. FIG. 3 Triangula! Specimen for T-Bend Test 6.2.2 Secure the specimen and bending die in a vise or holding jig (Fig. 2). Bend the specimen 180around the Jk in a smboth and uniform manner. 6.2.3 Examine the bend for cracking as in 6.1.4 and for loss of adhesion as in 6.1.5. 6.2.4 Express the T-bend to no cracking or' no pickoff as' the number of thickness around which the metal is being . bent equal to the thickness of the die. 7. Report 7.1 Report the following information: 7.1.1 Identification of the material, such as coil number' and location within the coil if the sample was, coated on a coil line, 7.1.2 The coating system, coating thickness, and applica tion and cure conditions, 7.1.3 The temperature at which the specimen is bent, 7.1.4 The bend direction--whether across or along th^ rolling direction of the sheet, 7.1.5 The minimum T-bend to no paint fracture, and > 7.1.6 The minimum T-bend to no pickoff. SPECitvltK- LENDING OIL 8. Precision3 8.1 On the basis of an interiaboratory study of this test, method, in which two operators in each of five laboratories tested panels coated with paints of different flexibility and adhesion, the standard deviation was found to be: Standard Deviation Aluminum Galvanized Steel T-bend to no fracture 0.55 1.33 T-bend to no pickoff 0,76 2.09 8.2 Based on these standard deviations, the following % FIG. 2 T-Bend Test Using a Die Around Which the Specimen is Bent 3 Supporting data are available from ASTM Headquarters. Request RR:P0l-* 1034. 664 r r rr DUP0502 97846 # D 4145 ,ff5j'eria should be used to judge the acceptability of results at 95% confidence level: S.2.1 Repeatability--Measurements obtained by two op- ^"ci.ttors in a single laboratory should be considered suspect if Aju'v differ by more than: b' Aluminum Galvanized Steel . T-bend to no fracture 0.4 1.8 T-bend to no pickoff 0.9 3.3 8.2.2 Reproducibility--Two measurements obtained in different laboratories, each the mean of measurements made by two operators within a laboratory,-, should be considered suspect if they differ by more than: T-bcnd to no fracture T-bend to no pickoff Galvanized Steel 2.5 10.1 1.8 10.6 The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of sue#? rights, are entltely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you feei that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 191$ Race St., Philadelphia, PA 19103. 665 DUP050297847 Designation: D 4146 - 83 (Reapproved 1989)* Standard Test Method for Formabiiity of Zinc-Rich Primer/Chromate Complex Coatings on Steel1 This standard is issued under the fixed designation D 4146; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicatestheyearoflast rcapprova! A superscript epsilon () indicates an editorial change since the last revision or reapproval. e 1 N' --Editorial changes were made throughout in March 1989. 1. Scope 1.1 This test method covers the evaluation of the formability and adhesion of factory applied zinc-rich primer/ chromate complex coatings on steel with thicknesses of0.025 to 0.05 in. (0.65 to 1.25 mm) typical of those used in the coil coating industry. 1.2 The degree of oil removal prior to forming, the techniques of taping, and differences in adhesive strength of the tape can affect the adhesion rating. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 7. 2. Referenced Documents 2.1 ASTM Standards: D3330 Test Method for Peel Adhesion of Pressure- Sensitive Tape at 180-Deg Angle2 2.2 Other Document-, Pictorial Standards ofCoating Defects1 * 3. Terminology 3.1 Description of Terms Specific to This Standard: 3.1.1 dome height--the height ofthe dome formed in the test. 3.1.2 indenting ball diameter--the diameter of the spherical-ended penetrator (ball) used to deform the specimen. 3.1.2.1 Discussion--The l5/s-in. (41-mm) diameter ball was selected because it minimizes the variability in the localized peak strain. This size ball is commercially available and is as large as most testing machines can accommodate. 3.1.3 percent strain--the percent elongation of scribed gage lengths after forming. For the draw height of 0.512 in. (13 mm), using a l5/s-in. diameter ball, the localized peak strain is about 19 % (see Fig. 1). 4. Summary of Test Method 4.1 A coated specimen is biaxially stretched a given distance in an appropriate machine, adhesive tape is applied to the deformed area (dome) and then pulled off, and the amount ofcoating removed is compared with a photograpine standard to determine the coating adhesion rating. 5. Significance and Use 5.1 The results of the combined deformation and tape 1 est are related to the ability of the coated metal to withstaui! stamping in factory applications. 5.2 This test can be used to control the manufacturing process or in development work to improve the product. 5.3 It should be recognized that variability in the results1,1 persist due to the test conditions and forming machinevariations. A TYPfCAL CURVE 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.53 on Coil Coated Metal, Current edition approved Oct. 28, 1983. Published January 1984. 2 Annual Book ofASTM Standards, Vol 15.09. 3 Copies of the picioria! photographic reference standard are contained in the publication Pictorial Standards ofCoatings Defects and may be obtained from the Federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. The silver halide gelatin photographs are intended to be the only primary reference standards for this test method. The reproductions of them in this test method are for the purpose of illustration only. 666 FIG. 1 Survey of Strain Over Biaxially Stretched Dome DUP050297848 D 4146 i Apparatus and Materials 16.1 Forming Machine, equipped with a spherical-ended Jnetrator to deform the specimen with appropriate dies, til the required height is obtained, and clamping arrange nt to hold the specimen with a minimum pressure of2000 (8.9 kN). 6.1.1 The speed of forming shall be between 0.2 and 1.0 ./min (4.8 and 25 mm/min). The speed is usually slowed to easure more accurately the final height as shown on the I indicator, but the final punch speed shall be controlled i}.24 in.(6 mm)/min maximum. f.2 Indenting Ball, with a diameter of 1% in. (41 mm), a .ckweil hardness number not less than 61 on the Rockwell ;scale (HRC), and a smooth surface finish not exceeding ' pin. (4 pm). The indenting ball shall not deform during test. The ball and holder shall move through the terline ofthe top and bottom dies. The ball shall be clean ^ free of oil, grease, oxide buildup, rust, dirt, nicks, or age. 1.3 Ball Holder, to hold the ball in its seat during the test, bt ball holders are removable so that other bail punch Jormation tests can be done in the same machine. 6.4 Upper and Lower Dies with a hardness of 56 HRC or Ter. Tlie upper die shall have an approach radius of 1525 0.002 in. (1,6 0.05 mm). The diameter of the ening in the upper and lower die shall be 1.64 in. (42 mm), most machines, these dies are removable. s5 Dial Indicator, riding on the surface of the forming et to monitor the movement of the penetrator (ball) and 'duated so that the displacement, or ball height, can be asured at least to 0.0025 in. (60 pm) but preferably to ,001 in. (25 pm). .6 Adhesive Tape, 1 in. (25 mm) wide, transparent, -tack, pressure-sensitive tape4 with an adhesive strength Steel of 45 oz/in. (50 g/mm) of width when tested in ordance with Test Method D 3330, and a tensile strength 28 lb/in. (500 g/mm) of width. 6,7 Photographic Standard5--Steps in rating from 10 `od, no removal) to 0 (poor, complete removal) to rate 'pally the adhesion of the coating after forming and tape oval by comparison with the adhesive-backed tape.: Hazards ",1 There are possible hazards to personnel when per iling tests on any hydraulic equipment. Stand free when ihine is operating. Sampling and Test Specimens 1 Sampling--The coated steel coil is cut, usually at the id or tail of the coil, into a sheet sample, which can be f iy handled. Specimen Size--The specimens may be square or tangular but not narrower than 3.5 in. (90 mm) in either IfiScotch Brand Transparent Tape No. 610, available from 3M Co., Commercial : Division, 3M Ceiller, St. Paul. MN 55101, has been found satisfactory for purpose. Equivalent material may be used. /The photographic reference standards that are part ofthis test method and are vic'ed in the Pictorial Standards ofCoaling Defects Handbook' are representa1:of the adhesion ratings. The photograph shown in Fig. 3 is for illustration poses only and should not be used for evaluation. Key 1 Test specimen 2 Spherical-ended penetrator (ball) 3 Ball holder 4 Clamp force (minimum) 5 Upper die; bore diameter 6 Lower die; bore diameter 7 Dome height 8 Upper die comer radius Dimensions Inch-Pound Metric -- in. -- 2000 Ibf 1.64 in.. 1.64 in. 0.512 in. 0.06251m -- 41 mm -- 8.9 kN 42 mm 42 mm 13. mm 1.6 mm FIG, 2 Tooling for Forming Test , dimension. Strips of full width of the coil can be tested if precautions are taken not to nick or damage the adjacent dome in the machine. 8.3 Specimen Thickness--Thicknesses should be 0.025 to 0.05 in. (0.64 to 1.25 mm). With thicknesses less than 0.025 in., fracture of the steel may occur, in which case the dome height can be reduced if agreed upon between the supplier and the user of the sheet product. When thicknesses greater than 0.05 in. are being tested, die modifications may be needed, but such modifications require agreement between the supplier and the user. 8.4 Test specimens shall be free of oil, grease, lubricants, rust/and burrs that may affect the holding pressures or dome height. 8.4.1 Typically a light spindle oil is applied to reduce corrosion on the uncoated side of the coil. 8.4.2 Remove oil, grease, and lubricants by one of two methods, as agreed upon between the supplier and the user. Either heat the specimens to 300F (I50C) for 30 min or wash them in a cleaning solution0, rinse with tap water, and dry. As the solution can become contaminated with oil, do not wash more than 50 panels per gallon of solution. 9. Procedure 9.1 Condition the specimens for at least 24 h at 73.5 3.5T (23 2C) and 50 5 % relative humidity before conducting the test, unless otherwise agreed.6 6 This is one cleaning solution that is used. Add 10 g of Car Wash Concentrate, a product of Borden Inc., Chemical Div., 180T E. Broad St., Columbus, OH 43215 (product formerly called DuPont No. 7 Car Wash), per gallon (2.6 g/L) of water at a temperature of I00*F (40'C). 667 DUP0502 97849 # D 4146 9.2 Place the specimen in the machine so that the coating to be tested will be on the convex side of the dome away from the punch. 9.3 With the ball touching the uncoated side of the specimen and the dial gage indicating zero penetration at the start of the test, indent the specimen with the ball to a distance of 0.512 in. (13 mm), ensuring that the hold-down pressure does not decrease during forming of the dome and that there is no evidence of slippage of the specimen under the hold-down dies during the test. The speed of forming the domes is done in accordance with 6.1.1. 9.4 Return the ball to the original position, remove the specimen from the machine, and lay it on a flat surface. 9.5 Apply the tape over the peak of the dome, press firmly, and then pull the tape from the dome at a fast, steady rate. The 1-in. (25-mm) wide tape will not fully cover the dome and will wrinkle at the edges. 9.6 Place the tape on a piece of white paper, compare the amount of coating on the tape with the photographic standard, and estimate coating adhesion to the nearest whole number. In Fig. 3, areas of darkness are coating removal so that a tape rating of No. 10 is perfect adhesion and No. 0 is complete removal ofthe coating. Wrinkles in the tape can be seen in the photographic standards as light areas. 9.7 Typically, a full-width specimen is cut from each coated coil and tested at three areas along the strip. Usually, domes are made at both edges and the center of the coated full width strip. 10. Report 10.1 Report the following information: 10.1.1 Identification of the material such as coil number and location of the specimen within the coil, 10.1.2 Specimen thickness, 10.1.3 Number of tests or domes evaluated, and 10.1.4 Adhesion rating including mean, range, or standard deviation, if applicable. 11. Precision 11.1 On the basis of an interlaboratory study of this test method, in which one operator in each of three laboratories tested five separate panels cut from the same coated steel, the within-laboratory standard deviation was 0.61 units with 12 df and the between-laboratory standard deviation was 0.35 with 2 df. Based on these standard deviations, the following criteria Should be used for judging the acceptability of results at the 95 % confidence level: 11.1.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 2 rating numbers. 11.1.2 Reproducibility--Two results, each the mean of two determinations, obtained by operators in different labo ratories should be considered suspect if they differ by more than 2.9 rating numbers. HATING TAPE STANDARD .5 12" D/>l L INDLNr AJlIPblGN TESt *i Y JUNE 1681 FIG. 3 Photographic Standard Adhesion Rating on Tape After Deformation The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either tor revision of this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments nave not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 668 DUP0502 97850 Designation: D 4147 - 82 (Reapproved 1987) Standard Practice for Applying Coil Coatings Using The Wire-Wound Drawdown > Bar1 2 *' This standard is issued under the fixed designation D 4147; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {<) indicates an editorial change since the last revision or reapproval. 3. Scope |l This practice covers a procedure for applying a ng film of uniform thickness on a flat panel using the @ire-wound drawdown bar. *il.2 This standard may involve hazardous materials, operMts, and equipment. This standard does not purport to m\ess all ofthe safetyproblems associated with its use. It is responsibility of the user of this standard to establish fopriate safety and health practices and determine the iUcability ofregulatory limitations prior to use. Summary of Practice r.rf.1 A flat panel is secured on a firm horizontal surface, tample amount of coating is poured across one end of the el and the drawdown bar placed behind the coating. The j is then drawn uniformly along the length of the panel Sard the operator to apply a uniform film. The dry film Ipcness obtained is dependent on the combination of the "j used, the volume solids of the coating, and the speed of > drawdown motion. J(Significance and Use ,1 This practice is useful in the laboratory to simulate Bl-coated films. {Apparatus fjft.l Wire-Wound Drawdown Bars2--A set of calibrated Unless steel wire-wound drawdown bars at least V2 in. (13 i$m) in diameter to prevent bowing during application. ' lliese bars are calibrated such that the diameter of the wire ||tmd on the bar controls thickness of the wet film applied, fche choice of specific drawdown bar is dependent on the dry gffim thickness required and the volume solids of the coating under test. 1 This practice is udder thejurisdiction of ASTM Committee D-l on Faint and ? 'Rtlated Coatings and Materials and is the direct responsibility of Subcommittee |p0l.53 on Factory-Prccoated Strip Metal. T Current edition approved June 25, 1982. Published September 1982. 2 Wire-wound drawdown bars may be obtained from R.D. Specialties, P.O. Box J06, Webster, N.Y. 14580, Paul N. Gardner Co., Inc., 21$ Commercial Blvd., iLauderdale-by-the-Sea, Fla. 33308, or the Leneta Co., P.O. Box 86, Ho-Ho-Kus, . 07423, or equivalent may be used. 4.2 Devices for Securing Panels: 4.2.1 Magnetic Ckuclc* for securing steel panels to elimi nate bowing. 4.2.2 Vacuum Plate4 for securing very lightweight nonmagnetic panels. 4.2.3 Tape for securing the top of thin-gage panels. 5. Safety Precautions 5.1 The flash points ofmost solvents used in coatings and related products are low enough that adequate ventilation is needed to avoid exceeding 25 % ofthe lower explosive limits of the solvent when preparing and baking the panels. As these solvents could be toxic, care should be taken to avoid inhalation of the vapors and unnecessary contact of the solvents with the skin. 6. Procedure 6.1 Deburr panels so edges are smooth. Secure a flat panel to be coated on a firm, uniform, level surface. To provide sufficient testing surface pour an ample amount of coating across the end of the panel. Place the drawdown bar behind the coating and pull into the coating. Rotate the drawdown bar 30 to 60in the coating to ensure complete wetting ofthe coating in the threads of the bar. Apply moderate pressure equally to both ends ofthe drawdown bar and hold it firmly without allowing rotation. Using only one pass, draw the bar along the length of and off the panel at a uniform speed so that a continuous film is produced. The drawdown speed is dependent on the rheology and type of the coating being used. Remove the coated panel and bake, force dry, or air dry the coating in accordance with its type so its dry film thickness can be measured. A heavier film thickness is obtained along the edges of the panel and possibly at the top of the panel where the coating was poured. For a two-coat system, the side edges must be trimmed to eliminate the heavier areas on the first coat before applying the second coat. J Magnetic chucks may be obtained from Brown & Sharpe Manufacturing, Co., Precision Park, North Kingstown, R.1.02852, or equivalent may be used. 4 Vacuum plate may be obtained from Paul N. Gardner Co., Inc., ZI8 Commercial Blvd., Lauderdale-by-the-Sea, Fla. 33308, or equivalent may be used. 669 m DUP0502 97851 # D 4147 The American Society ior Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressiy advised that determination of the validity of any such patent rights, and the risk of infringement oi such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will recalve careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. a 670 I DUP0502 97852 Designation: D 4206 - 89 Standard Test Method for Sustained Burning of Liquid Mixtures by the Setafiash Apparatus (Open Cup)1 This standard is issued under the fixed designation D 4206; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. INTRODUCTION This test method may be used in conjunction with a flash point determination. If the flash point of a mixture of flammable and nonflammable liquids or liquids of widely different flash points is below the upper limit of a flammability classification (for example, 100F specified by the U.S. Department of Transportation), this test may be conducted to determine the sustained burning characteristics of the mixture. This test method is a modification of the test for combustibility now incorporated as-Schedule 2 ofthe "Highly Flammable Liquids and Liquified Petroleum Gases Regulation, 1972" ofthe United Kingdom under The Factories Act, 1961, which is also issued as British Standard BS-3900, Part A-l 1, Small Scale Test for Combustibility. This sustained burning test was studied andproposed by the ASTM Coordinating Committee for Flash Point and Related Properties. The major purpose of this test is similar to that of the British test--to provide a method for determining the sustained burning characteristics by directly observing this property rather than by deducing them from the flash point, jgicope il This test method2 describes a procedure for deter-' ling the sustained burning characteristics of mixtures of pmable and nonflammable liquids and also mixtures gaining liquids with widely different flash points. 2 This standard should be used to measure and describe properties of materials, products, or assemblies in repse to heat and flame under controlled laboratory condi|ps and should not be used to describe or appraise.thefire yard orfire risk ofmaterials, products, or assemblies under .`ual fire conditions. However, results of this test may be ' as elements of a fire risk assessment which takes into nl all ofthefactors which are pertinent to an assessment efire hazard ofa particular end use. $ This standard may involve hazardous materiab, operfis, and equipment. This standard does not purport to 'ress all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish jropriate safety and health practices and determine the plicability ofregulatory limitations prior to use. ^Referenced Documents Si 1 British Standards? If This test method is under the jurisdiction ofASTM Committee D-l on Paint ^Related Coatings and Materials and is the direct responsibility of Subcomi|ee DO 1.22 on Health and Safety. 'urrent edition approved April 28, 1989. Published June 1989. Originally ' fished as D 4206 - 82. Last previous edition D 4206 - 82*1. iMcKelvie, A. N., "A Test for Ability to Support Combustion for Liquids ypuding Paints and Allied Products," Journal ofOil Co. Chemical Assoc., 1972> ||55, pp. 1086-1095. tfpAvailable from British Standards Institute, 2 Park St., London, England |3A2BS. BS-3900, Part A-11, Small Scale Test for Combustibility 3. Summary of Test Method 3.1 A block ofaluminum alloy, or other nonrusting metal of suitable heat conductivity, with a concave depression (called the well) is heated to the required temperature of 120F (49C). A standard source of flame, capable of being swung over the center of the well and at a given distance from it, is attached to the metal block. 3.2 Two millilitres of the product under test are trans ferred to the well. After the product has reached the stated temperature, the flame is passed over the well, held there for a specified time, and then removed. The time of sustained burning is then noted. 4. Significance and Use 4.1 Mixtures of flammable liquids and nonflammable liquids, such as an alcohol and water mixture, are classified by the U. S. Government by the definition of flammable liquid based on a closed-cup flash point method. Thus, mixtures may be classed as flammable even though they do not sustain burning. This test method determines the ability of a liquid mixture to sustain burning and, when used with a closed-cup flash point method, indicates the flammability characteristics of the mixture. 5. Apparatus 5.1 Setafiash Open-Cup Tester,A or an equivalent tester consisting of a 316 stainless steel block or other nonrusting4 4 Suitable apparatus is available from Erdco Engineering Corp., 721 Custer Ave., Evanston, JL 60204 or Stanhope-Seta Limited, Park Close, Englefield Egham, Surrey TW20 OXD, England. 671 DU PO 502 97853 A D 4206 block of suitable heat conductivity fitted with a concave depression or well (Note). The metal block has a thermom eter embedded in it. A small gas jet on a swivel is attached to the metal block. The exact dimensions of the metal block and its well, the gasjet and its positioning, and the embedded thermometer are shown in Fig. 1 and are specified in Annex AI. N' --While the Setaflash Open Cup Tester is generally made of an aluminum alloy, continued use of it for sustained burning tests rnay produce a carbon deposit in the well which may be difficult to remove without damaging the aluminum well. The stainless steel well may be cleaned with crocus cloth. 5.1.1 Gage--A metal strip, capable of checking the height ofthe gas jet above the top of the well lip (2.2 0.1 mm). 5.1.2 Hot Plate, fitted with a temperature-controlling device or other means of heating the metal block. 5.1.3 Stopwatch, or other-Suitable timing device* 5.2 Thermometer* 32 to 230F (-5 to 110C), traceable to the National Institute of Standards and Technology * 5.3 Graduated Pipet or Hypodermic Syringe,2 capable of delivering 2 0.1-mL. 6.1 Obtain a representative sample of the 'product under test, mixing it thoroughly, especially if it has a tendency to layer, and keep in an airtight container. 6.2 Because of the possibility of loss of volatile constitu ents, the sample should receive only the minimum treatment to assure uniformity. After removing the specimen, immedi ately close the sample container tightly to assure that no volatile flammable components escape from the container. (Otherwise a new sample may be necessary.if further testing is required.) 6.3 Do not open containers unnecessarily. Do not make transfers unless the sample temperature is at 100T (37.8C) or below, except for samples that are too viscous to be handled at that temperature. In these cases, transfer the samples at the lowest possible temperature at which the sample can be accurately measured into the cup. 6.4 Discard samples in leaky containers. 6.5 Do not store samples in plastic (polyethylene, poly propylene, etc.) bottles, since volatile material may diffusthrough the walls of the bottles. - 7. Correction for Barometric Pressure 7.1 When the barometric pressure differs from 760 mm Hg (101.3 kPa), determine the temperature at which the test should be conducted by the following equations: F = 120*F- 0.06 (760- P) C = 49C - 0.03 (760 - P) ' '/ = 120T- 0.42 (101.3 -B) C = 49"C-0.23 (101.3-if) where: F,C = temperatures to obtain the equivalent of 1207 (49C) at standard pressure, P barometric pressure, mm Hg, and B = barometric pressure, kPa. *.'9. Ill I IN Jggurns /'i/ii II K5il Mi. * KVi.f u SLOCK ASSEMBLY u 62.0 HA.--- 1 ALL DIMENSIONS IN MILUMET6PS FIG. 1 Setaflash Tester (Open Cup) 8. Procedure 8.1 Set up the apparatus (see 5.1) in a draft-free area. Plate the metal block on the hot plate fitted with a temperature-controlling device or heat the metal block h>, other suitable means so that the temperature is maintained".' I within 2F (l*C) of the temperature 120F (49C) Co p tog rected, if necessary, for the difference in pressure from 760'-5'" mm Hg <101.3 kPa). 8.2 After the cup is within 2`,F`(1C) of the correct tes, temperature, withdraw from the sample container a 2-mL, . specimen using the graduated syringe or pipet. Transfer the specimen to the well of the tester and immediately start the - J timing device. 8.3 Light the test flame with the jet in the "off" posil-cn 1 away from the well. Adjust the size of the flame so that il iispherical and approximately shi in. (4 mm) in diameter hv matching it to the -Va-in. diameter circle engraved on the surface of the tester. 8.4 After exactly 1 min (0 to +1 s) at which time the test portion will be deemed to have reached the test temperature as indicated by the thermometer embedded in the metal block, swing the test flame into a position exactly over the well. Hold it in this position for exactly 15 s and then return it to the "off" position. 8.5 Observe and time the duration of the burning of th^ specimen following the return of the flame to the "off" position. 8.6 Repeat the test with a fresh specimen and determine the mean time of burning. 672 DUPO 50297 854 ft B D 4206 Kiterpretation of Results jjl A product is considered to sustain burning if the jmen (a) ignites when the flame is over the well and ling is sustained for more than 15 s after it is removed, or flashes and burns when the test flame is in the "off" ^tisdion prior to swinging it over the well. 10.1.1 Identification of the material under test, 10.1.2 Test temperature and barometric pressure in milli metres of mercury (kilopascals), 10.1.3 Ifthe specimen burns less than 15 s. the actual time of burning, and 10.1.4 Statement of sustained burning characteristics. eport <&< >' ,0.1 Report the following information: 11.Precision 11.1 The precision ofthis test method will be determined. ANNEX Al. Dimensions of Tester (a) Meta! Block Details Diameter of block Height of block Diameter of flange Flange thickness Height of well "lip" above flange Diameter of well "lip" Spherical radius of well Depth of well Distance from top of block to thermometer hole Thermometer hple diameter (b) Test Gas Jet Details Outside diameter of Jet Jet end tapered to Bore of jet Length of jet (from center of axis to tip) Distance of axis from center of wall Flame gage ring diameter Helqht of let above top of welt "lip"/l "Swing" of jet (from stop to stop) Dimensions, mm 61.5-62.5 35.0-3.8.0 94,5-95.5 3.0 approx. 0.6-1.0 41.0 approx. 33.0-33.5 S.2-6.4 16.0-17.0 7.0 approx. Dimensions, mm 3.0-4.0 1.7-2.3 0.6-0.8 36.00-36.25 38.00-38.25 4.0 0.1 2.2 0.1 90 1 * Adjust with suitable g The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirety their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and It not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additions!standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you fee! that your comments have not received a lair hearing you should make your views known to the ASTM Committee oo Standards. 1916 Race SI. Philadelphia, PA 19103. 673 DUP0502 97855 (JjjjM Designation: D 4212 88 Standard Test Method for Viscosity by Dip-Type Viscosity Cups1 This standard is issued under the fixed designation D 4212; the number immediately following the designation indicates the year of original adoption or, in the case of revision, Ihe year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<} indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of viscosity of paints, varnishes, lacquers, and related liquid materials by dip-type viscosity cups. This test method is recommended only for viscosity control work within one plant or labora tory and should not be used to check compliance with specifications. 1.2 Viscosity cups are designed for testing of Newtonian and near-Newtonian liquids. If the test material is nonNewtonian, that is, shear-thinning or thixotropic, another method, such as Test Methods D 2196, should be used. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 1200 Test Method for Viscosity by Ford Viscosity Cup2 D2196 Test Methods for Rheological Properties of Non- Newtonian Materials by Rotational (Brookfield) Vis cometer2 D4287 Test Method for High Shear Viscosity Using the ICI Cone/Plate Viscometer2 E 1 Specification for ASTM Thermometers3 3. Terminology 3.1 Definitions: 3.1.1 near-Newtonian liquid--a liquid in which the varia tion of viscosity with shear rate is small and the effect on viscosity of mechanical disturbances such as stirring is negligible. 3.1.2 Newtonian liquid--a. liquid in which the viscosity is independent of the shear stress or shear rate. If the ratio of shear stress to shear rate is not constant, the liquid is non-Newtonian. 4. Summary of Test Method 4.1 The cup is completely immersed in the material to be tested, withdrawn, and the time for the material to flow through a hole in the base of the cup is measured. 5. Significance and Use 5.1 Viscosity is a measure of the fluidity of a material. Viscosity data are useful in the determination of the ease of stirring, pumping, dip coating, or other flow-related proper ties of paints and related fluids. 5.2 This type ofcup is used to measure viscosity because it is easy to use, robust, and may be used in tanks, reservoirs, and reactors. 5.3 There are other types of apparatus for measurim viscosity in the laboratory that provide better precision a in bias, including the Ford viscosity cup (Test Method D 120b) and the Brookfield viscometer (Test Methods D 2196). 5.4 Certain higher shear rate devices such as cone/plate viscometers (Test Method D 4287) provide more informa tion about sprayability, roll coatability, and other high-sheai rate related properties of coatings. V. 6. Apparatus 6.1 Zahn Viscosity Cup*--No. 1 through No. 5 Zahr. viscosity cups made of corrosion- and solvent-resistant materials. The capacity of the cup is nominally 44 mL, bi; may vary from 43 to 49 mL, depending on the manufu1-2 4 5 turer. A diagram of a Zahn cup is given in Fig. 1. The dimensions, including orifices, are only approximate because the cups are not made to one given specification. Each manufacturer produces a different cup and considerable;^ variation between batches from a given manufacturer been noted in the past. Thisas a major reason why Zahn curs should not be referenced in specifications between proi and user. (See Appendix X1 for additional information i Zahn Cups.) 6.1.1 Nominal Zahn cup orifice diameters are listed in Table Xl.l. Cup No. 1 with the smallest orifice is used determining the viscosity of thin-bodied materials. Cup No, 2 is for use with clears, lacquers, enamels, and press-sid: adjustment of flexographic inks; cups Nos. 3 and 4 are foe use with more viscous paints and inks (No. 3 for manufac turing of flexographic inks); and cup No. 5 is used for silk screen inks. 6.2 Shell Viscosity Cups--No. 1 through No. 6 Shell viscosity cups made of stainless steel with a capacity of 2' mL and a 1-in. (25-nvm) long capillary in the bottom and 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and is the direct responsibility of Subcommittee DO 1.24 on Physical Properties of Liquid Paints and Paint Materials. Current edition approved Dec. 30, 1988. Published April 1989. Originally published as D 4212 - 82. I> < <previous edition D 4212 - 82. 2 Annual Book ofASTM Standards, Vol 06.01. * Annual Book ofASTM Standards, Vol 14.03. 4 Zahn cups may be obtained from Paul N. Gardner Co., P.O, Box 10688, Pompano Beach, FL 33061 and from BYK-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 2(iyi0. It should be pointed out that cups from these sources arc not the same. Paul N. Gardner "Zahn signature" cup viscosities should not be compared to Pacific Scientific or G.E. cup viscosities oi to Paul N. Gardner "EZ" cup viscosities. 5 Shell cups may be obtained from the Norcross Corp., 255 Newtonville A* Newton, MA 02158. 674 DU P050297856 0.7 (18) 1.6 (41) i h',; D 4212 0.8 (20) 0.1 (3) 11.3 (33) ate aaear 1 (25)R hn> 0.7(17) jnl SPHERICAL R ml 10- :he (35) jse DIMENSIONS IN INCHES ok (MILLIMETERS IN PARENTHESES) 5le ibs fyfOTE--Dimensions are approximate only and may vary with the manufacturer and from batch to batch PS FIG. 1 ZahnCup in: porming to the dimensions shown in Fig. 2, 8. Temperature of Testing in k fit. Je fr b- 6.2.1 Nominal Shell cup orifice diameters are listed ip able XI.l. Cup Nos. 1 through 2>/2 are recommended for use with reduced rotogravure inks; No. 2 is for use with 'flexographic inks; Nos. 3 through 4 are used for industrial ie amels, lacquers, flexographic, and gravure inks; Nos. 5 and >6 ate used for heavy materials. o 3. Calibration Thermometer--ASTM Sayholt Viscosity 8.1 Measurements should be made at 77F (25C) unless otherwise specified. Temperature drift during the test should be kept to a minimum. The viscosities of paints and related materials are highly dependent on temperature. Differences in temperature between measurements can give substantially different viscosities (up to 5 % per F) . For careful work, the ftc Thermometer 17 having a range of 66 to 80F and temperature should be taken in the efflux stream, but for uhdivisions of 0.2F, or 17C having a range of 19 to 27"C process control (such as monitoring a dip tank), this is not nd subdivisions of 0.1C. both conforming to the require- necessary. 'it ents of Specification El. 8.2 Atemperature correction curve may be constructed > 6 3.1 For general operations, any thermometer with 1"C for each liquid by plotting viscosity (seconds) against temper subdivisions may be used. r,.4 Timer--Any timing device may be used provided that ature over the expected temperature range. With this curve, a viscosity determined at one measured temperature may be [the readings can be taken with a discrimination of 0.1 s or converted quickly to a viscosity at another temperature. Ktter. N' 1--When dip cups are used for original purposes, that is 7 Test Materials 7 1 The material to be tested should be visibly homoge thinning or monitoring of materials in tanks, coaters, etc., then temperature is not important. This is because the key to good operation is to maintain the fluid within a certain range of dip cup-seconds neous and free, from any foreign material or air bubbles. 675 WL DU P05 02 97857 ft D 4212 .13 (3.3) DU*'<32 [0.8) DEEP PLAT BOTTOMED HOLE regardless of the temperature of the plant or lab. 9. Checking and Calibration of Cups 9.1 Cups should be checked in accordance with the procedure described in Appendix X2. The frequency of this depends upon the amount of use and care that the individual cup receives. 9.2 Cups may be calibrated with standard oils according to the procedure in Appendix X3. However, because of the great temperature dependence of the viscosity of standard oils and the lack of adequate temperature control with dip cups, calibration is a difficult and often inaccurate procedure that must be done with great care. Because of the wide variability in Zahn cups, checking rather than calibration is recommended. 10. Procedure 10.1 Choose the proper cup so that the time of efflux will be between 20 and 80 s. See Table 1 for viscosity ranges for the various cups. 10.2 Immerse the cup in the container, which may be a can or beaker, but is more likely to be a thinning or mixing TABLE 1 Approximate Viscosity Ranges, cST (Roughly Corresponding to 20 to 80 s Row Time) Cup Number Zahn Cup Shell Cup \* 5-60 2-20 2 20-250 10-50 2Vz 20-80 3 100-600 30-120 3Vfe 40-170 4 200-1200 70-270 5 400-1600 125-520 6 320-1300 The lower limit for the Zahn No. 1 cup is 35 s rather than 20 s. tank or even a resin reactor. Stir or agitate the fluid well to give uniform temperature and density. Allow the cup to remain in the fluid for 1 to 5 min to attain thermal equilibrium. (Because of their greater mass, Shell cups should remain in the fluid for the full 5 min.) N' 2--Dip cups are not recommended for use with thixotropic (time dependent) materials but if used for them (such as gravure oti flexographic inks), more vigorous agitation will be necessary to break up' the structure before the measurement is made. 10.3 Lift the cup vertically out of the material in a quick, steady motion. As the top edge ofthe cup breaks the surface, start the timer. During the time of flow hold the cup t vertically no more than 6 in. above the level of the liquid. ' Stop the timer at the first definite break in the stream at lli base of the cup. The efflux time in seconds constitutes l viscosity. It is common to make only a single measureme but for greater precision and accuracy the mean of two more measurements should be taken. 11. Care of Cups ll.t Following each determination, clean the cup with suitable solvent and a soft brush. Use no metal tools ii^ contact with the instrument as nicks or wear of the drilled" orifice affect the accuracy of the cup. 12. Report 12.1 Report the efflux time to the nearest 0.2 s for Zahn or Shell cup No. ____, manufactured by , the, temperature of the fluid (and where measured, and whether the result is from a single measurement o t the mean oftwo of more measurements. 13. Precision and Bias 13.1 Dip cups are not precision instruments and should. 676 DU PO50297858 .^3 # D 4212 used for viscosity control at a given location only, '.(forever, if comparisons are made, cups from the same jlpnufacturer must be used. The following criteria can be pM for judging the acceptability of results at the 95 % ^uitidence level: Jgfe.l.l Zahn Cups--Precision was determined on the HGsis of an interlaboratory test in which six laboratories used Aen Zahn cups (all from the same set from the same 'trjanu facturer) to test eight paints covering a broad range of ,W.()Sities. The within-laboratory coefficient of variation was *' .3,7 r' and the between-laboratories coefficient of variation , 115%. Based on these coefficients the following criteria ` -hoi'Id be used for judging the acceptability of results at the H'% confidence level: 13.1.!.! Repeatability--Two results:, each the mean of measurements, obtained by the same operator should be Isidered suspect if they differ by more than 11 % of their 3pn value. |3.1.i.2 Reproducibility--Two results, each the mean of # measurements, obtained by operators in different labojdpks should be considered suspect if they differ by more B&' 33 % of their mean value. N' 3--Since the precision values were obtained under ideal conditions (a single set of cups), reproducibility in practice probably is poorer than that given (perhaps as bad as 50 %). 13.1.2 Shell Cups--Precision was determined on the basis of an interlaboratory test in which four, laboratories tested seven paints covering a broad range of viscosities. The within-laboratory coefficient of variation was 3.2 % and the between-laboratories coefficient of variation was 6.3 %. Based on these coefficients the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 13.1.2.1 Repeatability--Two results, each the mean of two measurements, obtained by the same operator should be considered suspect if they differ by more than 9 % of their mean value. 13.1.2.2 Reproducibility--Two results, each the mean of two measurements, obtained by operators in different labo ratories should be considered suspect if they differ by more than 18 % of their mean value. 14: Index Terms 14.1 This test method is indexed under the following terms: viscosity; dip cup(s); Zahn 'cup(s); Shell cup(s); flow cup(s). well to mp to termal cups ot: spit mre or rakup , )UK'k. lfuLC : cup [quid..1' at tiie"* :s the in nt, so ui APPENDIXES (Nonmandatory Information) XL ZAHN CUP DESIGN, MANUFACTURE, AND USE SCI. 1 Zahn cups were designed (and made by General jlcs-tric) as simple flow property devices for use in dip tanks, coat reservoirs, etc. They never were meant to be Ifcojnctcrs or to be used as such. Zahn cup use usually Trolves thinning or maintaining a coating, adhesive, or ink 'tcertain consistency (so many Zahn-seconds) regardless of jemperature. This is the beauty of dip cups. The operator iuows that his or her tank, bath, or coater runs well over a certain range of Zahn-seconds whether the plant temperature s SOT or 100T. The operator does whatever is necessary to JSep the fluid within the range. He or she does not care what 4jdic viscosity is at 25.0'C (77.0"F). XI.2 Because the Zahn cup patents have long since run out, the cups can be made by anyone. Each manufacturer makes cups that are somewhat different from those made by others. Considerable batch-to-batch difference from any given manufacturer has been seen in tlie past. Cup variations are not a problem for control of a bath or tank as long as new cups are compared to old ones for the Zahn cup-seconds operating window and a new window is established if necessary. However, cup differences cause great difficulty if cups are used to set producer-user specifications. Compari sons are almost impossible under such conditions. Uh .1 Is in" " ouIJ 677 m DU PO50297859 # D 4212 I X2. DIP CUP CHECKING PROCEDURES X2.1 Because Zahn cups vary with the manufacturer and batch, it is not possible to set up calibration equations that are applicable to all cups. Therefore, the only procedures that are recommended checking a cup against its original efflux time or comparing one cup against another. However, if a cup owner has an absolute compulsion to calibrate a Zahn cup, there are equations available (see X3). Shell cups may be checked by the same procedures as Zahn cups or may be calibrated. X2.2 Monitoring Cup Characteristics--A useful checking technique is to measure the efflux time for a new cup with a given standard oil, then check the cup periodically with the same oil at the same exact temperature to see whether the efflux time has changed. If the time changes drastically (greater than 20 %), the cup should be replaced. Ifthe change is small, the cup can be used as is or a correction can be made in subsequent efflux times of paints or other materials. The correction factor is equal to original oil efflux time divided by the current one. Recommended oils for such tests are given in Table X2.1. The viscosity of oils is very sensitive to temperature variations and, therefore, the temperature of the oil must be controlled closely during testing. It is recommended that the oil be held at the test temperature for at least 15 min prior to testing. X2.3 Comparing Cups--It sometimes is necessary to compare one Zahn cup with another in order to settle a dispute, determine whether a new cup will give similar times to an old one, etc. The most usual technique is to dip both TABLE X2.1 Viscosity Standards Recommended tor Checking Cups Cup Number Zahn 1 2 3 4 5 Shell 1 2 Vk 3 3Vz 4 5 6 ; Nominal Diameter-4 of Orifice, mm Standard Oil Number8 2.0 sto 2.7 S60 3.8 S200 4.3 S200 5.3 S350, S600 1.8 56 2.4 . S6. S10 2.7 S20 3.1 S20.S60 3.5 S60 3.8 S60 4.6 S80, S200 5.8 S200 Approximate oil ' Viscosity0 at 77"! (25C), CST 20 120 480 480 900,1600 9 9, 20 35 35,120 120 120 120. 480 480 A Information based on literature of cup manufacturers. 8 Certified kinematic viscosity standards (1-pt samples only) are available fro-" the Cannon Instrument Co., P.O. Box 16, State College, PA 16801. Oils from othi" sources, having known kinematic viscosities, may also bs used. Actual viscosity is noted on the label ol the standard. -5 'I II cups into the same container of standard oil at the same time and pull them out together, timing both of them. The efflux times are compared and a correction factor can be calcu lated. Sometimes paint or another material is substituted for the oil. i! i 1 X3. CALIBRATION OF DIP CUPS ii X3.1 Select the appropriate standard oil for the cup to be checked (see Table X2.1). X3.2 Bring the cup and the standard oil to a constant temperature as close as possible to 77.0F (25.0'C). Deter mine the time of efflux to the nearest 0.2 s using the procedure detailed in Section 10. Record the temperature of the efflux stream. If it is not 77"F, correct the viscosity of the standard oil to the actual temperature. X3.3 Convert the time of flow in seconds to kinematic viscosity as follows: V=K(t-c) where: F = kinematic viscosity, cST t = efflux time, s, and, K, c = appropriate constants (front Table X3.1). X3.3.1 These equations represent linear or relatively linear portions of the overall viscosity-time curves for the cups. The linear equations have been chosen because it is much more straightforward to make time corrections based on linear equations than on nonlinear ones. Zahn cup nonlinear equations that better fit viscosity curves for some TABLE X3.1 Constants for Use with Viscosity Formulas Cup K c Zahn 1 2 `3 4 5 Shell 1 2 3 3Vz 4 5 6 1.1 3.5 11.7 14.8 23 0.226 0.576 0.925 1.51 2.17 3.45 6.5 16.2 29 14 7.5 5 0 13 5 3 2 1.5 1 1 0.5 A Cup constants from Patton, T. C., Paint Flow and Pigment Dispersion, second edition, John Wiley & Sons, New York, 1979, p. 82. cups better may be found in the literature.6'7 No such equations for Shell cups have been published. X3.4 Calculate the correction factor by dividing the true kinematic viscosity of the standard oil by the kinematic 6 Euverard, M.> ASTM Bulletin, Vol 162, No. 67, October 1950. 7 Pierce, P. E., Journal ofPaint Technology, Vol 42, No. 533, 1969, p. 383. 678 DUP0502 97860 & jcosity calculated from the efflux time. This factor may then be used to correct viscosity readings taken with the cup. 4212 The product ofthe factor and an efflux time gives a corrected viscosity in Zahn or Shell seconds. The American Society for Testing and Materials takes no position respecting the validity of any patentrights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is sub/ect to revision at any time by the responsible technical committee and must be reviewed ovary five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, ft you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 679 DU P0502 97861 Designation: D 4213 - 87 Standard Test Method for Wet Abrasion Resistance of interior Paints1 This standard is issued under the fixed designation D 4213; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers an accelerated procedure for determining the resistance of interior paints to erosion caused by scrubbing. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 562 Test Method for Consistency of Paints Using the Stormer Viscometer2 D1 )93 Specification for Reagent Water3 D 1475 Test Method for Density of Paint, Varnish, Lac- guer, and Related Products2 D2369 Test Method for Volatile Content of Coatings2 D 2486 Test Method for Scrub Resistance ofInterior Latex Flat Wall Paints2 D2697 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings2 D2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings2 D3450 Test Method for Washability Properties ofInterior Architectural Coatings2 D 3980 Practice for Interlaboratory Testing of Paint and Related Materials2 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode4 3. Summary of Test Method 3.1 The test paint is applied to a black plastic panel. After conditioning, the coated panel is placed over a glass plate in a washability machine and scrubbed with a fine pore celluiosic sponge and an abrasive medium. The weight of the film eroded is determined by weighing the panel before and after the test, and the volume loss per stated number of cycles is calculated. 4. Significance and Use 4.1 Interior paints often become soiled especially near doorways, windows, and in work and play areas. This test 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.42 on Architectural Finishes. Current edition approved Dec. 14, 1987. Published February 1988. Originally published as D 4213 - 83. Last previous edition D42I3-83. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards. Vols 06.03 and 31.01. A Annual Book ofASTM Standards, Vol 15.05. method covers determination of the relative resistance of different interior paints to erosion when scrubbed. 4.2 Results obtained by this test method do not neces sarily represent the scrub resistance ofaged paint films, since scrub resistance may change with age. 4.3 Results obtained by this test method also do no: necessarily relate to relative ease of soil removal. 5. Apparatus 5.1 Wet Abrasion Test Apparatus.5 6 5.1.1 Accessory Apparatus {Fig. I).5 5.1.1.1 Sponge Holder,s sponge and sheet lead weights (total weight 500 10 g). s; 5.1.1.2 Glass Plate, measured to fit. 5.1.1.3 Gasketed Frame and Clamps. 5.2 Film Caster,7 having a 10 mil (250 pm) clearance and 5.5-in. (140-mm) path width. 5.3 Balance, weighing to 1 mg. 5.4 Oven, adjusted to 120 to 130F (50 to 55C). 6. Reagents and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests unless otherwise specified. Unless otherwise indicated, it is intended that all reagents shall conform to the Specifications of the Committee on Analytical Reagents ol the American Chemical Society, where such specif!cation', are available.8 Other grades may be used provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determi nation. 6.2 Purity of Water--Unless otherwise indicated, refeiences to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193. 6.3 Black Plastic Panels.9 6.4 Masking Tape. 6.5 Flannel Cloth. 5 The Gardner Abrasion Tester Model AG 8100 and accessory apparatu available from BYK.-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, $ilv< Spring, MD 20910 have been found satisfactory for this purpose. Other straight line wash testers may be adapted to meet the requirements of this test method. 6 This holder is also used as a brush holder in Test Method D 2486. It should not be confused with the sponge holder employed in Test Method D 3450. 7 The Dow film caster, available from the Gardner Laboratory Div., has bee found satisfactory for this purpose. e "Reagent Chemicals, American Chemical Society Specifications," Am Chemical Soc., Washington, DC. For suggestions on the testing of reagents n< listed by the American Chemical Society, see "Reagent Chemicals and Standards, by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "Unite States Pharmacopeia." 9 Leneta P-121-ION dull black plastic panels, 6'/2 by 17 in. by 10 mils (165 fc 432 by 0.25 mm) in size obtainable from the Lenela Co., P. O. Box 86, Ho-Hc K.us, NJ 07423, are suitable for the purpose. An equivalent may be used. 680 DU PO50297862 L CLEARANCE SPONGE HOLDER N' 1--When a referee test is made, prepare fresh medium or use standardized scrub medium from a previously unopened container that is no more than one year old. 6.8.1 Slowly add the hydroxyethylcellulose to the water while stirring mechanically. Stir until "uniform and then slowly add 2 to 3 drops of 28 % ammonium hydroxide solution while mixing and continue mixing until the solution turns clear. In the order shown, add the other ingredients separately, stirring continuously. Be sure each item is uni formly dispersed before adding the next one. Add the silica slowly to ensure uniform dispersion. Finally, add the preserv ative and adjust the pH with glacial acetic acid. GASKETED FRAME 7. Preparation of Apparatus 7.1 Scrub Test Apparatus--The scrub machine should be leveled before use and operated at 37 1 cpm. Before each test check the tightness of the motor belt or chain drive and alignment of the cables in both horizontal and vertical planes. Adjust tautness of the cables with the accessory spring scale to approximately 5 !b. 7.2 Cut the sponge to fit the standard brush holder, 3% by \lh by 1 s/s in. (95 by 38 by 40 mm). New sponges should be saturated with reagent water, wrung dry by hand and allowed to equilibrate in a constant temperature and humidity room for 24 h before being cut. 7.3 Brush Holder--Add sufficient weight to the holder in the form of sheet lead or other fiat weights to total 500 10 g including the sponge. METAL PAH FIG, 1 Accessory Apparatus for Scrub Test ( (> Detergent,10 6.7 Sponge*1 II fine pore, uncompressed sponge conrming to U.S. Federal Specification L-S-626, Type II, Fine re, Uncompressed. D 8 Scrub Medium12 (Note 1), consisting of the following: Water, reagent, Type IV i tydroxyethylccllulose13 Ammonium hydroxide, 28 % 1 letergent10 Trisodium phosphate, anhydrous Silica14 i \cetic acid, glacial Preservative15 49.4^ 0.8 2.0 2.0 45.0 0.7* 0.1 TOOE 4 Vary to achieve a viscosity from HO to 120 Krebs Units before use, as easured in accordance with Test Method D 562. n > iiv to achieve a pH from 9.5 to ID.O as measured in accordance with Test ethod E 70. I Octyl phenoxy polyethoxyethanol containing approximately ten moles of f\ n* oxide per mole has been found satisfactory. Triton X-100, obtainable " m Rohm and Haas Co.. Independence Square, Philadelphia, PA, is representa- of `his product An equivalent may be used. II Super-Cel Cellulose Sponge, Fine Pore #85, obtainable from American ' nge and Chamois Co., Inc., 47-100 34th St., Long Island City, NY l U01, has it und satisfactory for this purpose. An equivalent may be used. 1 Lmoratory standardized scrub medium is available from the Leneta Co. An bivalent may be used. 8. Procedure 8.1 Stir the material under test thoroughly and strain to remove all skins and particles. Clean the top ofthe glass plate (or preferably suction plate) and both sides of the black plastic panel to be sure they are free of specks. Place the black panel on the plate and tape one end to the plate. Smooth the panel along the plate by rubbing with flannel, creating static electricity to improve adhesion to the plate. 8.2 Drawdown the paint on the panel using the 10-mil (0.25-mm) side of the film caster, starting as close to the taped end of the panel as possible (should be less than Vi in. (13 mm) from the taped end of the panel). The time of application should be fairly slow--3 to 4 s from end to end--to prevent formation of pinholes or holidays in the film. Air dry in a horizontal position for seven days in an open room, preferably kept at 73 3.5F (23 2C) and 50 5 % relative humidity. 8.3 After the specified drying time, cut off the top % in. (20 mm) of the panel, preferably with a paper cutter to 13 Hydroxcthylceliulose having a molar substitution (MS) value of 1.8 to 2.5 and a viscosity of a 2 % solution in the range qf 4400 to 6500 cPs., Cellosize QP-4400, obtainable from Union Carbide Co., Chemicals Div., 270 Park Ave., New York, NY 10017, has been found satisfactory for this purpose, as well as Natrosol 250 MR obtainable from Hercules Inc., 910 Market St., Wilmington, DE 19899. 14 This silica is an amorphous grade of 99+ % silicon dioxide giving a pH of 6.8 to 7.2 in reagent water. Average particle size is 2.95 pm with 92 % being less than 50 pm and surface area of 7600 cm2/g. Silica No. 22 obtainable from Whittaker, Clark and Daniels, Inc., 100 Church St., New York.. NY 10007, has been found satisfactory for this purpose. An equivalent may be used. 15 1,3,5 iriethyl hexahydro-sym-triazine (Vancide TH) obtainable from R. T. Vanderbilt Co., 30 Winfield St., Norwolk, CT 06855, has been found satisfactory. An equivalent may be used. 6S1 Bsaii DUPO 502 97863  D 4213 ensure a smooth straight edge. The film should now cover the panel uniformly along its entire length, exactly 16`A in. (413 mm). The panel may now be cut in half, length-wise? so that duplicate tests can be run. Roll the test panels into the shape of a cylinder to fit the balance pan, fasten the ends together with a paper clip and weigh to 1 mg. Record this as Weight A. Remove the clip and carefully unroll the panel. Save the paper clip for later weighings. Avoid any damage to the film after weighing. 8.4 Clean the glass plate and set it in the pan of the scrub test apparatus. Place the test panel, with painted side up, over the glass plate so that the test area is level. Pre-wet the gasket ofthe frame (if frame is to be used), and wipe dry before use. Place the frame over the drawdown and clamp in place. Clamps should be tight enough to ensure close contact but not tight enough to cause warping of the panel. 8.5 Place the sponge in reagent water and allow to remain for 30 min. Remove, hand squeeze dry, and insert in the weighted holder. Stir the scrub medium and spread 10 g evenly over the face of the sponge. Place the sponge at the end ofthe panel and wet the path of the sponge on the panel with 5 mL of water. 8.6 Note counter reading on scrub test apparatus and start the test. Make sure the sponge travels only over the test panel and only over the coated portion of the panel, and that sponge and holder are level during run. If the sponge and carriage tend to tilt sidewise, twist the cable in the direction in which the holder is tilting to impart an opposing torque to the sponge and holder enabling them to ride upright. 8.6.1 Caution--Cables should not be twisted more than three or four times. Excessive twisting in the direction opposite to that used to form the cable can cause unraveling of cable strands. 8.7 After each 100 cycles examine the panel for erosion through to the substrate. If cut-through is evident, stop the test and record the number of cycles. Otherwise continue until 400 cycles, at which time add 10 g of stirred medium to the sponge again and 5 mL of water to the panel, and continue testing to a maximum of 1000 cycles. Add 10 g scrub medium and 5 mL deionized water at the end of every 400 cycles. 8.7.1 In instances where cut-through is observed, repeat the test using the other half of the test chart and stop at least 100 cycles short of the previously noted cut-through point. It is important not to erode the film to the point where the substrate shows through since this will cause an erroneous result. 8.8 Rinse off the panel with tap water making sure all scrub medium has been removed, brushing gently with a soft camel hair brush to facilitate removal of the scrub medium. Blot the panel (do not rub) with paper towels, allow to air dry for 30 min, and then place flat in the oven at 120 to 130F (50 to 55C) for 30 min. Remove and allow to equilibriate for 15 to 20 min preferably in a conditioned room, or if necessary at ambient conditions surrounding the balance. Roll the panel into a cylinder, dip the edges together with the paper clip used in the initial weighing, and weigh to 1 mg. Record this as Weight B. Then calculate the Erosion Rate C in accordance with 9.1. 8.9 Between runs, rinse the sponge thoroughly to remove as much detergent as possible, soak the sponge in reagent water before the next test, and then proceed as in 8.5. 8.10 Make three drawdowns from each sample. Test two panels (four tests), then calculate the mean value of C and report this value unless any of the results differ by more than 25 % ofthe mean. Ifthey do, test the third panel and include the two results in the mean unless one of the results is obviously discrepant, in which case it should be discarded. N' 2--See Table 3 of Practice D 3980 for limits used in rejecting extreme values. 8.11 Determine the density (D) of the paint in g/mL, in accordance with Test Method D 1475. 8.12 Determine the percent nonvolatile by weight, (W), of the paint, in accordance with Test Method D 2369. 9. Calculation 9.1 Determine the total weight loss in milligrams for each panel by subtracting B from A. Divide the weight loss by the number of cycles and multiply by 100 to determine the erosion rate C expressed as milligrams lost per 100 cycles, thus: (A - B) x 100 number of cycles 9,2 Calculate V, the percent nonvolatile by volume of the paint as follows: 9.2.1 Water-borne Paints--V = 100 -- D(100 -- W) 9.2.2 Solvent-borne Paints--V - 100 -- 1.2823(100 - W) 9.3 Calculate the erosion rate in terms of wet film volume, thus: microlitres _ 100 C 100 cycles -- WD N' 3--This value relates to the whole paint and is thus analogous, though inversely, to the cycles-to-failure values of Test Method D 24Sf 9.4 Calculate the erosion rate in terms of dry film volume,, thus: microlitres _ CV 100*cycles ~ WD N' 4--This value relates to the nonvolatile portion of the paint The film volume in the equation is exclusive of interstitial air, whether due to vesiculated beads or ordinary porosity. 10. Report 10.1 Report the following information: 10.1.1 Erosion rate of the equivalent wet film tot* microlitres/100 cycles, as calculated in 9.3. 10.1.2 Erosion rate of the dry film in microlitres/100 cycles, as calculated in 9.4 10.1.3 Number of tests. 10.1.4 Number of cycles at which any erosion to tht substrate initially occurred. 10.1.5 Any deviations from the standard procedure. 11. Precision 11.1 In an interlaboratory study of this test method in' which operators in six laboratories tested three latex coatings covering a range of pigment volume concentrations, the'within-laboratory coefficient of vartiation was found to 5.6 % and the between-laboratories coefficient 9.4 %. Based 682 DUP0502 97864 *0 an *c IS in -! ft ie tc # D 4213 these coefficients of variation the following criteria should used for judging the acceptability of results at the 95 % idence level: [1.1.1 Repeatability--Two results, each the mean of two it tests, obtained by the same operator, should be lidered suspect if they differ by more than 18 % of the .n. 11.1.2 Reproducibility--Two results, each the mean of repeat tests, obtained by operators in different laborato ries, should be considered suspect if they differ by more than 30 % of the mean. 12. Indexing Terms 12.1 This test method is indexed under the following terms: abrasion (of paints/related coatings); interior paints/ coatings; resistance--abrasion (of paints/related coatings); resistance--scrubbing; weight--weight loss. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and .toif not revised, either reapproved, or withdrawn. Your comments are invited either for revision of this standard.or foradditionalstandards and should fee addressed ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouid make your views known to the ASTM Committee on Standards, 1916 Pace St.f Philadelphia, PA 19103. 683 DU PO 502 97 865 Designation: D 4214 - 89 a-; Standard Test Methods for Evaluating the Degree of Chalking of Exterior Paint Films1 ' jr1- This standard is issued under the fixed designation D 4214; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. This standard has been approvedfor use by agencies of the Department ofDefense. Consult the DoD Index of Specifications and Standardsfor the specific year ofissue which has been adopted by the Department ofDefense. 1. Scope 1.1 These test methods cover the evaluation of the degree of chalking on white or lightly tinted exterior paint films. It describes the procedures recommended for transferring the chalk to a fabric or fingertip, which is then compared to photographic reference standards, or in the case of adhesive tapes, compared to a reflectance table or photographic ref erence standards, to determine the degree of chalking. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D659 Method of Evaluating Degree of Chalking of Exterior Paints2 3 4 D 662 Test Method for Evaluating Degree of Erosion of Exterior Paints2 D1150 Single and Multi-Panel Forms for Recording Results of Exposure Tests of Paints2,3 E 97 Test Method for Directional Reflectance Factor, 45-Deg O-Deg, of Opaque Specimens by Broad-Band Filter Reflectometry2 2.2 Other Document: Pictorial Standards of Coating Defects* 3. Terminology 3.1 Definition: 3.1.1 chalking--the formation on a pigmented coating of a friable powder evolved from the film itself at or just beneath the surface. 1 These? test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coalings and Materials and are the direct responsibility of Subcommittee D01.27 on Accelerated Testing. Current edition approved March 31, 1989. Published June 1989. Originally published as D 4214-82. Last previous edition D4214-82 2 Annual Book ofASTM Standards, Vol 06.01. 3 These record sheets may be obtained from ASTM, 1916 Race St., Philadelphia, PA 19103 {request Adjunct Nos. 12-411500-11 and 12-411500-21} and from the Federation of Societies for Coatings Technology, 492 Norristown Rd.> Blue Bell, PA 19422. 4 Copies of the pictorial photographic reference standards applicable to Tesl Method D 659 are contained in the publication Pictorial Standards of Coalings Defects and may be obtained from the Federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. 4. Significance and Use 4.1 The procedures provide a broader range of techniques and photographic references to evaluate chalking of exteriopaints than that in Method D 659 and are thus an extension of that method. 5. Type of Chalking 5.1 Only one type of chalking is recognized, as defined in Section 3. 6. Use of Photographic Reference Standards 6.1 The photographic reference standards that are part of this test method are representative of the degrees of chalkinjon a paint film. The photographs shown in Figs. 1 and 2 ari for illustration purposes only and should not be used foevaluation. 6.2 The use of photographic reference standards illus trated in Figs. 1, 2, 3, and 4 requires the following precau tions: 6.2.1 The degree ofchalking will vary over any given area. Therefore, an average portion ofthe coating should be evalu ated. On large surfaces, it is recommended that the rating be made at several locations and the mean and range reported 6.2.2 It is difficult to make readings on a windy day and making readings at such time should be avoided. It should 'l also be noted that rain, snow, or moisture in any form v tl remove chalk so that readings should be made after a pet too of clear weather and when the surface is dry. 6.2.3 Chalking and erosion (Note 1) are closely rela' 1 and erosion is a result of chalking failure. However, the rate j of chalking as measured by these test methods, and the nut of erosion may not be comparable because some pigment" combinations tend to retain chalk on the surface while othecj pigment combinations exert a self-cleaning action by naturali| means. N' l--For the evaluation of erosion, see Test Method D 662 6.3 Records may be kept on forms such as shown in 1 tc 3, according to Standard D 1150, or other inspection forms The reporting of the results shall include the informal tor given in Section 10. 6.4 When this test method is referenced in specifications fij for performance, the permissible degree of chalking established between the producer and the user. vs IS -jw is M $j 4>Vt :3 ? Steif 7. Recommended Procedures--Wood Substrates 7.1 Test Method A--Method D 659: 7.1.1 Material--Fabric, as agreed upon between the pro ducer, user, or other interested parties, to rub against tt - ... 684 DU PO 502 97866 # D 4214 No. 8 nii 1 No. 6 No. 4 No. 2 FIG. 1 Photographic Reference Standard No. 1--Test Method D 659 Yace being tested. Black wool felt, velvet, and velveteen vc picven particularly effective. f7 1 - Procedure--Wrap the fabric around the index fin,ir then apply it with medium pressure to the coating observation. Rotate the finger through an angle of holding the fabric so it also rotates. Remove the fabric ^compare the , spot of chalk on it with Photographic rence Standard No. 1. ^2 Test Method B--Stroke Method: `f.Z 1 Material--Fabric as in 7.1.1. tj,? 2 Procedure--Wrap the fabric around the index fin' ip. hen make a 3-in. (75-tnm) stroke with medium svure on the coating under observation. Remove the u ' and compare the spot of chalk on it with Photographic erence Standard No. 1. S-1 Test Method C--Wet Finger Method: jJ 1 I Procedure--Moisten a fingertip and with medium gffiure make one continuous rub 2 to 2'h in. (50 to 65 t) in length on the surface under test; Compare the utf on the finger.with Photographic Reference Standard i; This test method can be used quite effectively by enenced operators and is recommended mainly for he-field evaluation when use of one of the other methods 'impractical. IirCD Jpcommended Procedures--Metallic Substrate--IndusTrial, Automotive, and Coil Coatings '` '8 1 Test Method C--Wet Finger Method--See 7.3. l Test Method D--Transparent Tape Method? 2.1 Materials: jg 2.1.1 Cellulose Adhesive Tape,6 Vi in. (13 mm) wide, Ssure-sensitive. fe, t .2 Eraser, V4 in. (20 mm), wrapped with cellophane 2.1.3 Masking Tape, lh in. (13 mm) wide. <'8 2.1.4 Plastic Sheet Protector, clear. FIG. 2 Photographic Reference Standard No. 2--Verfinstituut TNO 8.2.1.5 Photographic Reference Standard No. 2, TNO.7 8.2.1.6 Reflectance Standard, polished black glass. 8.2.1.7 Reflectance Standard, white tile. ' Permission to include this method is provided as a courtesy of NL Chemicals, J&ofT1Mills tid., Hightstown, NJ 08520. ** Permacel 404 manufactured by Permacel, !nc.. Route I, New Brunswick, NJ and Scotch Brand tape No. 600 manufactured by The 3M Company, n.k-v,iag Systems, 3M Center, Bldg. 230F267, St. Paul, MN 55144, have been gjltfd suitable for the purpose. 7 The TNO Method and photographic reference standard are provided as a courtesy of Ver/inslituut TNO Paint Research Institute TNO, Schoemakeretraat 97, Delft, Nederland. The original source of the photographic reference standard illustrated in Rg. 2 is the Paint Research Institute, TNO. The A.STM numerical rating of chalking shown on the photographic reference standard is opposite to the original TNO scale. 685 B-K s ? 1' s" DU PO 502 97867 TAPE CHALK RATING WORKSHEET Reflectance Method Client Name___ Order #________ Radiation to date. Measurements Avg/% Corrected Value Rating TAPE CHALK RATING WORKSHEET Rari<tno9 Hqthod Client Base ____ or4w * .... /CrWag. Radiation to date bJC M'f'/e%/ t/l/ Heftourements _Si!sat______ &J/H.____ J>2S ft Sheet-_& 1st Sat 2nd Set S.1*0 *.c s Sheet Tape & Sheet 1st Set 2nd Set 1 2 3 4 5 6 7 8 9 10 Tape 8 Sheet Sheet , Date ----------------------- Inspected by-------------N' --Label sample numbers, apply Initial blank tape, and proceed with tape specimens of the samples. FIG. 3 Example of Worksheet N' 2--The black reference standard is necessary as the back ground for this measurement, since the reflectance of black paper is too high. Reflectometers (tristimulus colorimeters), with 0 to 45 degree geometry, use the Y value. 8.2.2 Optional Materials: 8.2.2.1 China Marker, black. 8.2.2.2 Razor Blade. 8.2.3 Preparation: 8.2.3.1 Separately mount and apply two 11-in. (279-mm) pieces of masking tape along the right side ofthe clear plastic sheet cover leaving 1 lU in. (32 mm) of space between the pieces (see Fig. 3). 8.2.3.2 Remove a 2 in. (50 mm) long piece of '/i in. (13 _____. -JLX&tk-- ,,,, 1 .___4/,,. 10 tf.tl .._____fti rt.46lA ____ff Sheet ___ e-a-tr mux sneer , v?, d3if N' --The cut-out section Is (or Illustration purposes only. The labeling (ch na marker) may be removed by ribbing the sheet wilh a clean tissue Or doth. FIG. 4 Completed Worksheet mm) cellulose, pressure-sensitive adhesive tape from the roll, place it across the masking strips, and adhere it to the sheet using a %-in. (20-mm) eraser, wrapped with cellophane tape Label this tape "blank" on the clear plastic sheet cover. A black china marker has been found useful for this purpose N' 3--The average reflectance measurements of the initial and ending "blank" tapes less the correction value for the clear plastic sheet divided by tOO are used to verify a rating of 10 using Table I.8 8.2.4 Procedure: 8.2.4.1 Apply a 2 in. (50 mm) lung piece of Vi in. ([3 mini wide tape to the surface being rated. Rub ten times with moderate pressure using the covered eraser, to remove all bubbles and prevent scratching. Remove the tape from the surface and adhere it to the sheet by rubbing with the eraser. Label specimens using a black china marker. Place succes sive tapes vertically adjacent to previous tapes, separated by `/s in. (3 mm). Follow the instructions given in 8.2.3.2, ano place the final "blank" tape across the masking tape strips and label "blank" on the clear sheet. When completed, use a razor blade to cut along the inside edges of the masking tape, cutting through the adhesive tapes. The removal of the masking tape will leave only the tapes to be measured and evaluated with the sample number of each tape listed on the 8Kronos-Titan Table for Chalk Rating from Reflectance Reading using the Transparent Tope Method is provided as a courtesy of Kronos-Titan GMbH, Leverkusen, West Germany, The original source of Table 1 is Kronos-Titan GMbH. 1 686 DU PO 502 97868 1 sling (chi |oth the roll, he ilicetj, ne tariff t3miui es with*' < ,. j oni th.eraser success, ? ateit b, .2, and' e strips i, use a1, ig tare, of the ed and . on the # D 4214 TABLE 1 Chalk Rating from Reflectance Reading'1 ipr ft t r , Reflectance Range 0-0.038 0,0381-0.044 0.0441-0.054 0.0541-0.062 0.0621-0.072 0.0721-0.082 0.0821-0.095 0.0951-0.105 0.1051-0.120 0.1201-0.131 0.1311-0.150 0.1501-0.165 0.1651-0.190 0.1901-0,210 0.2101-0.235 0.2351-0.260 0.2601-0.286 0.2861-0.310 0.3101-0.340 0.3401-0.366 >0.366 Chalk Rating 10 9.5 9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0 jfTjWs table is based upon a correlation between tape reflectance measurefjftS'and visual evaluations of the same tape compared to the photographic Hdjrds prepared by Kronos-Titan. It (see worksheet example in Fig. 4). Before proceeding, Iqk to ensure all sample numbers have been recorded on fleet. jd.4.2 Insert the Vh-in. (13-mm) aperture and calibrate Iteflectometer according to the manufacturer's instrucsetting the reflectometer for zero reflectance using black reflectance standard and standardizing with the lie reflectance standard and record the values. Refer to |i Method E 97 should there be any question on the let procedure to follow in the calibration of the instru- |. 2.5 Reflectometer Measurements: 12.5.1 Leave the transparent tapes mounted on the clear (tic sheet. Remove the black paper that may have been Sited behind the sheet and fold back the unused portion sheet. Measure the reflectance of the clear plastic sheet ig the black reflectance standard of the instrument (Note a backing or background and record its value. Move the (ft until the first tape is exposed to the light source with Adhesive side toward the light and the black reflectance idard behind the area being measured, and record the ue. .2.5.2 Continue this procedure until ten tapes have been Jfasured, then check reflectance values for the white and j|fk standards. If no changes have occurred, proceed with fasurements. If values have changed, restandardize and ord values before proceeding to the remaining tapes. Bowing the final tape measurement, record reflectance dues ofthe clear plastic sheet cover and the white and black fectance standards. '8.2.5.3 Subtract the mean reflectance value of the sheet m each reading, enter on worksheet form (Fig. 4), or other prm used, and determine from Table Is the chalk rating (flue of each tape to the nearest 0.5 unit. Record the rating the worksheet or other form. The worksheet form (Fig. 4), inserted into the plastic sheet protector with a black back ground gives a clear permanent record of these measure ments and evaluations. 8.2.6 These tape chalks may also be compared to Photo graphic Reference Standard No. 2 as'an alternative proce dure. 8.3 Test Method E-TNO Method: 8.3.1 Materials: 8.3.1.1 Photographic Reference Standard No. 2 for the determination ofchalking, consisting of a photograph of five strips of tape mounted on a black background, numbered 0, 2,4, 6, and 8, and varying in this order from white to almost black. The numerical rating of chalking shown on the photographic reference standard is opposite of the original TNO Scale. 8.3.1.2 Polyethylene Tape,9 transparent, 1-in. (25-mm) wide. 8.3.1.3 Black Velvet, dull black with a short pile and without a tendency to crush, size approximately 8 by 12 in. (200 by 300 mm), mounted on a flat substrate. Place adjacent to the standard for the ratings. 8.3.2 Procedure--Apply a piece of tape, approximately 4-in. (100-mm) long, to the coating by uniform gentle pressure of the finger, remove the tape, and lay it with the adhesive side on the piece of velvet. Under diffused light compare the tape on the black velvet with PhotogfaphiC Reference Standard No. 2, and determine which of the five grades most closely matches the whiteness of the adhering pigment. If the degree of chalking is obviously between two adjacent grades, select the intermediate odd number as the chalk rating. 8.3.3 Chalk ratings may also be determined by following the procedures of 8.2.3 and comparing to the values showil in Table 1. The use of the worksheet form shown in Figs;'3 and 4 may be used as a permanent record. 9. Recommendations 9.1 The procedures recommended for various substrates and coatings are based upon the results obtained in interlaboratory testing. The selection of the method to be used is subject to agreement between producer and user! 10. Report /. 10.1 A record of the test method used, the rating,,.panel number, and other pertinent information must becfearly shown on the inspection report for each evaluation.' The report form may be in accordance with Standard D ifeo or other form agreed upon between the producer and thctiser. 10.2 The pertinent information should include: date of inspection, date of exposure start, purchase order number of testing organization, duration, remarks about unusual weather, etc., the name of the person making the insfpition, and other information agreed upon between the producer and the seller. 9 Sellotape 1401, Transparent Polythene Electrical, manufactured l$$jellotape Products Ltd., Edgeware, Middlesex, England has been found suitafjg; for this purpose. 687 DU P050297869 # D 4214 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are express/y adv/sed that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject fo rev/s/on at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreepprcved or withdrawn. Yourcomments are invited either for revision ofthis standard or for add/ti'onaf standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at e meeting of the responsible technical committee, which you may attend. It you feel tftal your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, PA 19103. 688 DUP050297870 Designation: D 4227 - 83 (Reapproved 1989) Standard Practice for Qualification of Journeyman Painters for Application of Coatings to Concrete Surfaces of Safety-Related Areas in fjfg|fj Nuclear Facilities1 *J8{' This standard is issued under the fixed designation D4227; the number immediately following the designation indicates the year of origmal.adoption or, in the case of revision, the year oflast revision, A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. npe ffihis practice provides a standard qualifying method ourneyman painters to verify their proficiency and * to attain the required quality for application of "fled coatings to concrete surfaces in safety-related areas 'nuclear facility. , , Variations or simplifications of the practice set forth ;i` may be appropriate for special coating work such as Ipaiance. It is not the intent of this practice to mandate liar basis for all qualifications. J, Evaluation of the journeyman painter being qualified 'oordance with this practice, shall be by qualified agents eified in 4,1. Reports shall be prepared as specified in t >i i 5. and qualification as specified in Section 6. It is the intent of this practice to judge only the ability v journeyman painter to apply specified coatings with poper tools and equipment. This standard may involve hazardous materials, oper and equipment. This standard does not purport to s all ofthe safety problems associated with its use. It is esponsibility of the user of this standard to establish priate safety and health practices and determine the ability ofregulatory limitations prior to use. -finitions journeyman painter--an individual who has worked e painting trade sufficiently long enough to master the f all applicable tools and the materials being applied. 2 qualifying agents--the designated representatives of ij|vner or of the coating organization, or both, who have eient experience in the practical application and evaluaof coating applied to concrete surfaces of a nuclear governing documents--technical specifications, jobsite "'ures, and reference documents. -{ plication of Coatings !! This practice requires the journeyman painter to ' the specified coating in conformance to the governing Uments to a test area similar to that detailed in Figs. 1 *2. Jl. 1 Ceiling Section--Beginning at the wall line, one 5 >-ft (1.5 by 1.5-m) coating. 3.1.2 Wall Section--Beginning at the floor line, one 5 by 5-ft (1.5 by 1.5-m) coating. 3.1.3 Floor Section--Beginning at the wall line and con necting with the wall section, one 5 by 5-ft (1.5 by 1.5-m) coating. 3.2 This practice requires the journeyman painter per form the application using the proper technique and appli cation equipment consistent with the governing documents. 3.3 The surfaces of the concrete test area shall be prepared in accordance with the governing documents. 3.4 The journeyman painter shall demonstrate the ability to apply the specified coating to a uniform dry film thickness in accordance with the governing documents, as evaluated by the qualifying agents. 3.5 When desired by the owner, one of the test surfaces may include embedded steel. 3.6 If a coating system specified requires a primer, inter mediate, and finish coat, treat each coat as a separate application, allowing a specified drying time before applying each succeeding coat. 3.7 The journeyman painter shall be provided with the following: p.This practice is under the jurisdiction of ASTM Committee D-33 on (Active Coating and Lining Work for Power Generating Facilities and is the ct responsibility of Subcommittee D33.07 on Application. Current edition approved April 6, 1983. Published June 1983. 689 DUP050297871 # D 4227 56 7 9 10 11 13 ' 1 15 5'-o" a 12 16 S-O" FIG. 3 Location of Wet-Film Thickness Readings 3.7.1 Information regarding the specified coating material(s), including wet and dry film thickness required, and all other information contained in the governing documents for the coating system being applied. 3.7.2 Coating materials properly mixed in accordance with the governing documents and ready for application. 3.7.3 The necessary equipment for the proper application of the specified coating. 3.7.4 Miscellaneous equipment, brushes, and thinners required for cleaning the equipment after completion of the test. 3.7.5 A practice area to adjust and test the equipment prior to performing the test. 3.7.6 All necessary safety equipment. 3.7.7 Wet-film thickness gage for verifying the coating thickness during application. 3.8 The journeyman painter shall use the wet-film thick ness gage furnished to determine coating thickness buildup during application. Material thickness is one of the criteria for evaluation, 4. Evaluation of Coating Application 4.1 Evaluation of the journeyman painter shall be made by two qualifying agents. Only one qualifying agent can be production-related. 4.2 The qualifying agents shall be capable of answering technical questions requested by the journeyman painter relating to the application ofthe specified coating material(s) The qualifying agents shall be thoroughly familiar with ihe specified coating materials) and acceptance criteria and shall be aware of any difficulties in applying the coating to any surface. 4.3 The qualifying agents shall have a wet-film gage of (he same type used by the journeyman painter. 4.4 The qualifying agents shall take approximately if, wet-film thickness readings on the test areas. These readings shall be recorded as specified in Section 5. The wet-film thickness readings shall be used to verify the specif ^ dry-film thickness requirements and uniformity of appliestion. The number and location of readings shall be a indicated on Fig. 3. 4.5 The journeyman painter and the qualifying agents shall understand the required dry-film thickness range r,quirements of the governing documents before any coatiur are applied. 4.6 The qualifying agent shall inspect the finished surfaic to verify that it conforms to the requirements of uw governing documents. A description ofthe appearance ofthe? completed applied coating shall be recorded on the form- r shown in Fig. 4. 5. Report 5.1 The qualifying agents shall use a report form simil.ir to that in Fig. 4 to record wet-film thickness readings" specified in 4.4, and the appearance ofthe completed coaling.surface as specified in 4.6. 5.2 The qualifying agents and journeyman painter slid1 sign the report form. Test Application of Coating to Standard Concrete Test Areas by Journeyman Painter for Qualification for Coating of Concrete Surfaces In Safety-Related Areas of Nuclear Facilities Type of Recording Instrument for Wet-Film (WFT) Thickness:_______ --'! WFT Reading No. 1. 2. 3. 4. 5. 6. 7. 8. Flow Test Area Wall Test Area Ceiling Test Area 10. 11. 12. 13. 14. 15. 16. Description of Materials:.. Qualifying AgentQualifying Agent:Journeyman:_____ FIG. 4 Record Form for Test Application 690 DU P050297872 Hyman's Name: (Site):_____ 'ng Agents: y System:_______________ fuifacturen ________________ ? of Application Equipment: . `inents: --------------------------- Journeyman Paints Qualification for Application of Coatings to Concrete Surfaces of Safety-Related Areas of Nuclear Facilities Representing: . Representing: Itie above applicant has been qualified as a Journeyman Painter for the application of the above coatings for concrete surfaces of safety-related areas of nuclear > Qualifying Agent:Qualifying Agent:_ Joumeymanu- FIG, 5 Qualification Form 8 A copy of the report shall become a permanent part of uality assurance file for the nuclear project for which 'ourneyman painter is qualifying. 'A copy of the report shall be given to the qualifying eyman painter. `tial Qualification 1 The qualifying agents shall prepare a qualification similar to Fig. 5. The qualification form shall state the g materials used and the application equipment used 'test. The qualifying agents and the journeyman painter j sign the qualification form. 3 A copy of the qualification form shall become a anent part of the quality assurance file for the nuclear ect for which the journeyman painter is qualified. A copy of qualification form shall be given to the Reyman painter. 7. Requalification 7.1 The owner or his designated representative may deter mine the degree of requalification to be permitted, as well as the acceptance of previously qualified journeyman painters based on time interval since the date of the qualification and provided the same coating materials and application proce dures are used. Note the acceptance of previous qualification in the quality assurance file for the project. 8. Limited Qualifications--Touch Up and Repair 8.1 Limited qualifications can be accomplished using only areas representative ofthe actual plant surfaces, even though they do not include all areas represented by Figs. 1 and 2. 9. Limited Qualifications--Brushes, Rollers, Squeegees, or Other Special Tools 9.1 Limited qualifications for special application tools may be required on certain projects. When such limited qualification is performed,.the limitations shall be noted on the records for qualification and application. The American Sactely tor Testing end Materials takes no position respecting the validity of eny patent rights asserted In connection with any item mentioned In this standard. Users of this standard are express*/ advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible teohnlcal committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Yovr comments are invited either lorrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feeI that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. u 691 DUPO 502 97873 Designation: D 4228 - 83 (Reapproved 1989) Standard Practice for Qualification of Journeyman Painters for Application of Coatings to Steel Surfaces of Safety-Related Areas in Nuclear Facilities1 This standard is issued under the fixed designation D 4228; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {<) indicates an editorial change since the Iasi revision or reapproval. 1. Scope 1.1 This practice provides a standard Qualifying method for journeyman painters to verify their proficiency and ability to attain the required quality for application of specified coatings to steel surfaces in safety-related areas in a nuclear facility. 1.2 Variations or simplifications of the practice set forth herein may be appropriate for special coating work such as maintenance or qualifications of equipment suppliers shop personnel. It is not the intent of this practice to mandate a singular basis for all qualifications. 1.3 Evaluation of the journeyman painter being qualified in accordance with this practice, shall be by qualified agents as specified in 4.1. Reports shall be prepared as specified in Section 5, and certification as specified in Section 6. 1-4 It is the intent of this practice to judge only the ability of the journeyman painter to apply specified coatings with the proper tools and equipment. 1.5 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregidatory limitations prior to use. 2. Definitions 2.1 journeyman painter--an individual who has worked in the painting trade sufficiently long enough to master the use of all applicable tools and the materials being applied. 2.2 qualifying agents--the designated representatives of the owner or of the coating organization, or both, who have sufficient experience in the practical application and evalua tion of coatings applied to steel surfaces of a nuclear facility. 2.3 governing documents--technical specifications, jobsite procedures, and reference documents. 3. Application of Coatings 3.1 This practice requires the journeyman painter to apply the specified coating in conformance to the governing documents to a test panel similar to that detailed in Fig. 1. This panel is typical of the panel used for qualification, and may be modified to suit site configurations. 3.2 This practice requires the journeyman painter to ` This practice is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities and is the direct responsibility of Subcommittee D33.07 on Application. Current edition approved April 6, 1983. Published June 1983. perform the application using die proper technique and application equipment consistent with the specified coating materials. 3.3 The surfaces of the test panel shall be prepared in accordance with the governing documents. 3.4 Place the test panel approximately 12 in. (305 mm) above ground level and at approximately 30 from the5' vertical plane, with the complex side up. This will simulate'! the types of difficult coating situations encountered byil journeyman painters in a nuclear facility. 3.5 The journeyman painter shall demonstrate his ability5' to apply the specified coating to a uniform dry-film thickness in accordance with the governing documents, as evaluated! by the qualifying agents. 3.6 Allow required drying as prescribed by the governing! documents prior to taking the dry-film thickness reading of; the applied coating.-If a coating'system specified requires a primer, intermediate, and finish coat, treat each coat as a separate application, allowing a specified drying time before; inspecting each completed coat. 3.7 The journeyman painter shall be provided with the following: - 3.7.1 Information regarding the specified coating mate?; rial(s), including wet and dry film thickness required, and all other information contained in the governing documents fcSj the coating system being applied. I 3.7.2 Coating materials properly mixed in accordance with the governing documents and ready for application, j 3.7.3 The necessary equipment for the proper application! of the specified coating. ;j 3.7.4 Miscellaneous equipment, brushes, and thinnerij required for cleaning the equipment after completion of the ; test. J 3.7.5 A practice area to adjust and test the equipmettjjj pxior to performing the test. I 3.7.6 All necessary safety equipment. 3.7.7 Wet-film thickness gage fortesting the coating! thickness during application, where applicable. ; 4. Evaluation of Coating Application 4.1 Evaluation of the journeyman painter shall be made by two qualifying agents. Only one qualifying agent can be production-related. 4.2 The qualifying agents shall be capable of answering technical questions requested by the journeyman painter, relating to the application of the specified coating material(s}.i The qualifying agents shall be thoroughly familiar with the specified coating materiai(s) and acceptance criteria and shall; 692 DUPO 502 97874 D 4228 completed applied coating and dry film thickness shall be recorded on form Fig. 3. 6" diameter pipe l1-6 long 5. Report 5.1 The qualifying agents shall use a report form similar to that in Fig. 2 to record dry-film thickness readings 5'-0" specified in 4.4, and the appearance ofthe completed'coating surface as specified in 4.6. '' 5.2 The qualifying agents and journeyman painter shall sign the report form. 5.3 A copy of the report shall become a permanent part of the quality assurance file for the nuclear project for which the journeyman painter is qualifying. 5.4 A copy of the report shall be given to the qualifying journeyman painter. FIG. 1 Test Panel--Complex Side l&ware of any difficulties in applying the coating to any Igce. IIS The qualifying agents shall have a wet-film gage of the fje type used by the journeyman painter, as well as a brated magnetic-type dry-film thickness gage. 1.4 The qualifying .agents shall take dry-film .thickness . dings on all areas of the test panel, except nuts and bolts. e readings shall be recorded as specified in Section 5. jit-film readings may be used to check the journeyman r's progress during application. The dry-film thickness |fding shall be used to verify the specified dry-film thick- requirements and uniformity of application. The Saber and location of readings shall be as indicated on Fig. jp.5 The journeyman painter and the qualifying agents ill understand the required dry-film thickness range re tirements of the governing documents before any coatings eapplied, |46 The qualifying agent shall inspect the finished surface verify that it conforms to the requirements of the .verning documents. A description of the appearance of the 6. Initial Qualification 6.1 The qualifying agents shall prepare a form similar to Fig. 3. The qualification form shall state the coating mate rials used and the application equipment used in the test. 6;2v The qualifying agents and the journeyman painter shall sign the qualification folm. 613' A copy of the qualification form shall become a permanent part of the quality assurance file for the nuclear project, for. tyhiefi' the journeyman painter.is qualified. 6.4 A copy of the qualification form shall be given to the journeyman painter, 7. Requalification 7.1 The owner or his designated representative may deter mine the degree of requalification to be permitted, as well as the acceptance of previously qualified journeyman painters based on time interval since the date of the qualification form and provided the same coating materials and applica tion procedures are used. Note the acceptance of previous qualification in the quality assurance file or the project. * 8. Limited Qualifications--Touch Up and Repair 8.1 limited qualifications can be accomplished using only areas representative of the actual plant surfaces, even though they do not include all areas represented in Fig. 1. Tast Application of Coating to Standard Steel Test Panel by Journeyman Painter for Qualification for Coating of Steel Surfaces in Safety-Related Areas of Nuclear Facilities jjjpeyman:_____________________________ _ Readings Wet Dry Implex Side: * Seam: " Bar l^te: [ascription of Finished Surface: kipT Range: Qualifying Agent: Qualifying Agent: Journeyman: ____ FIG. 2 Record Form for Test Application 693 DUP050297875 Journeyman's Name: Location (Site): 1. p Coating System: Manufacturer: Comments: D4228 Journeyman Painter Qualification for Application of Coatings to Steel Surfaces of Safety-Related Areas of Nuclear Facilities Qualifying Agents: ~ ~ The above applicant has been certified as a Journeyman Painter for the application of the above coatings for steel surfaces of safety-related areas of nuclear 1 ties. Date: Qualifying Agent: Journeyman: .. Qualifying Agent:. FIG. 3 Qualification Form 9. Limited Qualifications--Brushes, Rollers, or, Other Spe cial Tools 9.1 Limited qualifications for special application tools may be required on certain projects. When such liir iii i qualification is performed, the limitations shall be noted on the records for qualification and application. TheAmerican Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned In this standard. Users ofthis standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at eny time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Yourcomments are invited either farrevision ofthis standard orhradditional standards and should be addressed to AS7M Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, ll you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7976 Race St., Philadelphia, PA 19103. r r 694 DU PO 50297876 Designation: D 4236 - 91 Standard Practice for Labeling Art Materials for Chronic Health Hazards1 This standard is issued under the fixed designation D 4236; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. INTRODUCTION Uninformed or careless use of some art material products can give rise to health hazards, either acute or chronic, or both. Specific and readily available warnings are needed to help protect users of any age. One way to disseminate such information is to provide appropriate precautionary labeling on art material products. Labeling for acute health hazards, including those associated with art materials, is being addressed by such requirements as the U.S. Consumer Product Safety Act, the Federal Hazardous Substances Act, and the like. There are presently no specific national standards for labeling art materials with respect to chronic health hazards. This practice is intended to provide a standard for developing precautionary labels concerning chronic health hazards related to the use of art materials. It is further intended to have the adaptability necessary to keep labels current with existing scientific and medical knowledge, as well as in conformity with Other precautionary labeling requirements, both acute and chronic, thereby avoiding unnecessary confusion by users with respect to other precautionary labeling. Scope 111 This practice describes a procedure fof developing autionary labels for art materials and provides hazard precautionary statements based upon knowledge that ; in the scientific and medical communities. This plac- ; concerns those chronic health hazards known to be assowiih a product or product component(s), when the Iponent(s) is present in,a physical form, volume, or conatration that in the opinion of a toxicologist (see 2.1.11) 5 the potential to produce a chronic adverse health effect(s), jj.,2 This practice applies, exclusively to art materials ckaged in sizes intended for individual users of any age or : participating in a small group. Labeling determinations shall consider reasonable eable use or misuse. The responsibility for precaulabeling rests with the producer or repackager who ets the materials for art or craft use. '1.4 This practice does not specify test methods for deter- ng whether a substance or product presents chronic Ihealth hazards. rl.5 This practice does not apply to products appropriately I labeled for known chronic health hazards in accordance with [chemical substance labeling standards and practices, such as another national consensus standard, existing labeling stats utes, regulations, or guidelines. 1.6 Since knowledge about chronic health hazards is incomplete and warnings cannot cover all uses of any prodmet, it is not possible for precautionary labeling to ensure 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee L> )1.57 on Artist Paints and Related Materials. Current edition approved Sept. 15, J991. Published November 1991. Origi. nally published as D 4236 - 83. Last previous edition D 4236 - 89. completely safe use of an art product. 1.7 Manufacturers or repackagers may wish to determine individually or collectively precautionary labeling for art materials in accordance with this practice. Compliance may be certified by a certifying organization. Guidelines for a certifying organization are given in Appendix XL 1.8 This standard does not purport to address all of the safely problems, if any, associated with its use. ft is the responsibility ofthe user ofthis standard to establish appropriate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Terminology 2.1 Descriptions of Terms Specific to This Standard: 2.1.1 analytical laboratory--a laboratory having per sonnel and apparatus capable of performing quantitative or qualitative analyses of art materials, which may yield infor mation that is'used by a toxicologist for evaluation of potentially hazardous materials. 2.1.2 art material or art material product--any raw or processed material, or manufactured product, marketed or represented by the producer or repackager as intended for and suitable for users as defined herein. 2.1.3 bioavailability--the extent that a substance can be absorbed in a biologically active form. 2.1.4 chronic adverse health effect(s)--a persistent toxic effect(s) that develops over time from a single, prolonged, or repeated exposure to a substance. This effect may result from exposure(s) to a substance that can, in humans, cause sterility, birth defects, harm to a developing fetus or to a nursing infant, cancer, allergenic sensitization, damage to the nervous system, or a persistent adverse effect to any other organ system. 695 DU P0502 97877 # D 4236 2.1.5 chronic health hazard(s) (hereafter referred to as "chronic hazard")--a health risk to humans, resultant from exposure to a substance that may cause a chronic adverse health effect. 2.1.6 label--a display of written, printed, or graphic matter upon the immediate container of any art material product. When the product is unpackaged, or is not pack aged in an immediate container intended or suitable for delivery to users, the label can be a display of such matter directly upon the article involved or upon a tag or other suitable labeling device attached to the art material. 2.1.7 producer--the person or entity who manufactures, processes, or imports an art material. . 2.1.8 repackager--the person or entity who obtains mate rials from producers and without making changes in such materials puts them in containers intended for sale as art materials to users. 2.1.9 sensitizer--a substance known to cause, through an allergic process, a chronic adverse health efFect which be comes evident in a significant number of people on re- exposure to the same substance. 2.1.10 toxic--applies to any substance that is likely to produce personal injury or illness to humans through inges tion, inhalation, or skin contact. - 2.1.11 toxicologist--an individual who through .educa tion, training, and experience has expertise in the field of toxicology, as it relates to human exposure, and is either a toxicologist or physician certified by a nationally recognized certification board. 2.1.12 users--.artists or crafts people of any age. who create, or recreate in a limited number! largely by hand, works which may or may not have a practical use, but in which aesthetic considerations are paramount. 3. Requirements 3.1 To conform to this voluntary practice the producer or repackager of art materials shall submit art material product formulation(s) or reformulation(s) to a toxicologist for re view, such review to be in accordance with Section 4 of this practice. The toxicologist shall be required to keep product formulation(s) confidential. 3.1.1 Unless otherwise agreed in writing by the producer or repackager, no one other than the toxicologist shall have access to the formulation(s); except that the toxicologist shall furnish a patient's physician, on a confidential basis, the information necessary to diagnose or treat cases of exposure or accidental ingestion. 3.2 To conform to this practice, the producer or repack ager, upon advice given by a toxicologist in accordance with Section 4 of this practice, shall adopt precautionary labeling in accordance with Section 5 of this practice and based upon generally accepted, well-established evidence that a compo nent substance(s) is known to cause chronic adverse health effects. 3.3 To conform to this practice, labeling shall be parallel to, conform to, and minimally include any labeling practices prescribed by U.S. federal and state statutes or regulations and shall not diminish the effect of required acute toxicity warnings. 3.4 To conform to this practice, the producer or repack ager shall supply a poison exposure management informa tion source2 the generic formulation information required for dissemination to poison control centers or provide a 24-h cost-free telephone number to poison control centers. 3.5 To conform to this practice, the producer or repack ager shall have a toxicologist review as necessary, but at least every 5 years, art material product formulation(s) and associated Iabel(s) based upon the then current, generally accepted, well-established scientific knowledge. 3.6 Statement of Conformance--"Conforms to ASTM Practice D 4236," or "Conforms to ASTM D 4236," or "Conforms to the health requirements of ASTM D 4236." This statement may be combined with other conformance statements. The purpose of the conformance statement is to inform the purchaser, at the time of purchase, of tL product's compliance with the standard. To accomplish this purpose the conformance statement should appear wheat- er practical on the product; however, it shall also be acceptable to place the statement on one or more of the following: (a) the individual product package, (b) a display or sign at the point of purchase, (e) separate explanatory literature avail able on request at the point of purchase, (d) a response to a formal request for bid or proposal. . 4. Determination of Labeling 4.1 An art material is considered to have the potential Vr producing chronic adverse health effects if any customary oc reasonably foreseeable use can result in a chronic hazard 4.2 In making the determination a toxicologist(s) shall take into account the following: 4.2.1 Current chemical composition of the art material, supplied by an analytical laboratory or by an industrial chemist on behalf of a manufacturer or repackager. 4.2.2 Current generally accepted, well-established scien tific knowledge of the chronic toxic potential of each component and the total formulation. 4.2.3 Specific physical and chemical form of the aft material product, bioavailability, concentration, and the'1 amount of each potentially chronic toxic component fou.io in the formulation. 4.2.4 Reasonably foreseeable uses of the art matenJ product as determined by consultation with users and other, individuals who are experienced in use of the material(s)f such as teachers, or by market studies, unless such use information has previously been determined with respect tiTf the specific art material(s) under review. 4.2.5 Potential for known synergism and antagonism e , the various components of the formulation. 4.2.6 Potentially chronic adverse health effects of decom-"1 position or combustion products, if known, from any reasonably foreseeable use of the hazardous art material product. 4.2.7 Opinions of various regulatory agencies and scieu- j3| tific bodies, including the International Agency for Research on Cancer and the National Cancer Institute, on the poten tial for chronic adverse health effects of the various compo- ' nents of the formulation. 2 Two of the larger poison exposure management information sources are ThS>` Rocky Mountain Poison Control Center, West 8th and Cherokee. Demur, CO 80204; and the National Poison Center Network, 125 De Solo St., Pittsburgh, PA 15213. 696 DUP050297878 I. # D 4236 luired 24-h ten:ach Of 3. Based upon the conclusion reached in conformance review determinations set forth herein the toxicolo- j|s) shall recommend precautionary labeling consistent i Section 5 of this practice. ' Labeling Practices ' 1 Signal Word: ' 1.1 When a signal word for an acute hazard(s) is ndated and a chronic hazard(s) exists, the signal word the thht for the acute hazard. '.1.2 When only a chronic hazard(s) exists, the signal prd WARNING shall be used. 1.1.3 The signal word shall be prominently visible and set bold capitals in a size equal to or greater than the sent of potential chronic hazards. List of Potentially Chronic Hazards--Potentially onic hazards, as determined under the procedures of jj,on 4, shall be stated substantially in accordance with the tgihents listed in Annex A1 of this practice. Potentially |nic hazards noted shall be those that are clinically ficant and that might be expected with any reasonably eable use of the art material. The hazards should be 1 in the order of relative descending severity, p Name of Chronically Hazardous Component(s)--AW ffionents and known decomposition products of the tulation with a potential for chronic hazards, as deter- under the procedures of Section 4, shall be listed .eminently. Genetically equivalent names may be used. |5.4 Safe Handling Instructions--Appropriate pre.caun iry statements as to work practices, personal protection, ventilation requirements shall be used substantially orming with those listed in Annex A2 of this practice. 5.5 List of Sensitizing Components--To protect users i known sensitizers found within art materials, each label ; contain a list of those sensitizers present in sufficient counts to contribute significantly to a known skin or iratory sensitization. > 6 Combined Statements--If an art material contains Jie than one component capable of causing a chronic arse health effect, or if a single chemical can cause several ent chronic adverse health effects, the potential effects be.combined into one statement. Information Sources--In addition to an appropriate |ephone number, the precautionary label shall contain a unent identifying a source for additional health informa tion substantially in conformance with one of the phrases listed below; 5.7.1 For more health information--(24-h cost-free tele phone number), or * 5.7.2 For further health information call a poison control center. 5.8 Labeling Content, Product Size--An art material produces) in a container larger in size than one fluid ounce (30 mL) (if the product is sold by volume) or one ounce net weight (28 g) (if the product is sold by weight) shall have full precautionary labeling, as generally described in Section 5 of this practice. An art material product(s) in a container equal to or smaller than one fluid ounce or one ounce net weight shall have a label that includes a signal word in conformance with 5.1 of this practice and a list of potentially harmful or sensitizing components in conformance with 5.3 and 5.5 of this practice. 5.9 The information described in Section 5 must appear (1) on the outside container or wrapper, if any, unless it is easily legible through the outside container or wrapper and (2) on all accompanying literature where there are directions for use, written or otherwise. In a case where one or more individual product(s), which require warning labels under Sections 4 and 5, are packed within a point of sale package which obscures the warning statement(s), the point of sale package shall carry the signal word conforming to 5.1 of this practice and the following wording: "Contains: (list haz ardous produces)) that may be harmful if misused. Read cautions on individual containers carefully. Keep out of the reach of children." 5.10 Statements required under Sections 4 and 5 must be in the English language and located prominently in con spicuous and legible type in contrast by topography, layout, or color with other printed matter on the label. 5.11 Supplemental Information--Where appropriate, more detailed technical information that relates to chronic hazard(s), such as physical properties, decomposition prod ucts, detailed safety instructions, or disposal recommenda tions, shall be included in supplemental documents, such as Material Safety Data Sheets, technical brochures, technical data sheets etc. 6. Keywords 6.1 art materials; chronic toxicity; craft materials; health labeling; precautionary statements; warning statements ANNEXES (Mandatory Information) Al. CHRONIC HAZARD STATEMENTS ; M VY CAUSE STERILITY. ( UNTACT MAY CAUSE PERMANENT EYE 1 'MAGE. MAY BE HARMFUL BY BREATHING VAPORS/ >iNrs. ma y b e h a r mf u l if s w a l l o w e d . 'MAY BE HARMFUL BY SKIN CONTACT. Ma y p r o d u c e b ir t h d e f e c t s in t h e d e v e l o p in g FETUS. MAY BE EXCRETED IN HUMAN MILK. MAY CAUSE HARM TO THE NURSING INFANT. CANCER AGENT! EXPOSURE MAY PRODUCE CANCER. 697 1 DUP050297879 T # D 4236 CANCER AGENT BASED ON TESTS WITH LABORA HEATING/COMBUSTION MAY CAUSE ,,i HAZ TORY ANIMALS. ARDOUS DECOMPOSITION PRODUCTS. POSSIBLE CANCER AGENT BASED ON TESTS MAY CAUSE (SPECIFIC EFFECT) OF (SPECIFY WITH LABORATORY ANIMALS. MAY PRODUCE ALLERGIC REACTION BY INGES TION/INHALATION/SKIN CONTACT. MAY PRODUCE NUMBNESS OR WEAKNESS IN THE EXTREMITIES. EXPOSURE MAY CAUSE (SPECIFY THE ORGAN). CANCER AGENT! EXPOSURE BY (SPECIFIC ROUTE) MAY PRODUCE CANCER. MAY CAUSE HARM TO THE DEVELOPING FETUS EXPOSURE MAY RESULT IN NAUSEA, HEAD- ACHE, CONFUSION OR INSTABILITY. MAY CAUSE DAMAGE TO RED BLOOD CELLS ORGAN(S))DAMAGE. WITH REDUCED ABILITY TO CARRY OXYGEN. A3. PRECAUTIONARY STATEMENTS Keep out of reach of children. When using do not eat, drink, or smoke. Wash hands immediately after use. Avoid inhalation/ingestion/skin contact. Avoid fumes from combustion. Keep container tightly dosed when not in use. Store in well-ventilated area. Wear protective clothing (specify type). Wear protective goggles/face shield. Wear NIOSH3-certified mask for dusts/mists/fumes. Wear NIOSH-certified respirator with an appropriate cartridge for (specify). Wear NIOSH-certified supplied-air respirator. 3 U. S. National Institute ofOccupational Safety and Health. Use window exhaust fan to remove vapors and ensure adequate cross ventilation. (Specify explosion-proof if neces sary.) Do not heat above (specify temperature) without adequate ventilation. Use (specify type) focal exhausting hood. . Do not use/mix with (specify material). Do not dry grind. Do not spray apply. If pregnant or contemplating pregnancy, use only under: professional supervision. Avoid using/do not use if pregnant (or contemplating pregnancy). Not for use by children. Avoid breathing dust. Use in glove box. APPENDIX (Nonriumdatory Information) XL GUIDELINES FOR A CERTIFYING ORGANIZATION XI.I The term certifying organization, as used in these guidelines, refers to an organization or an institute that, after assuring that all provisions are met, certifies that an art material does conform to the labeling requirements of this practice. XL2 The certifying body may be funded by member manufacturers, but should include users or their representa tives, as well as manufacturers' chemisls, on its technical and certifying committees. X1.3 Representative samples of art materials, labeled as conforming to this practice and bought at retail, should be analyzed at random and from time to time by an analytical laboratory to ensure they are the same as the formulation used by the toxicologists) for determining labeling require ments. X1.4 The methods used by the toxicologist(s) in revi|i| and determination of the need and content of precautionary.] labeling for potentially chronic adverse health effects rbci" 1 be periodically reviewed by an advisory board composed' not less than three or more than five toxicologists, at least-) one of whom is certified in toxicology by a nationally ! recognized certification board. XL5 In cases where there is disagreement by participating producers or participating users, with the determination U the toxicologist(s), there should be a method whereby tf' toxicologist's decision can be presented to the advisory board of toxicologists for arbitration. The American Society for Testing and Materials takes no position respecting tha validity of any patent rights asserted in connection with any item mentioned in this standard. Users ot this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standardis subject to revision at any time by the responslhie technical committee and must bs reviewed every live years and it not revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should da addressed to ASW Headquaners. Your comments will receive careful consideration at a meeting of the responsible technical committee. which you may attend. If you feet thet your comments hove not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 191C3. 698 DUPO50297880 Designation: D 4256 - 89 h az- pec if y `ECIFIC FETUS. HEAD. CELLS :n . ensure f neces... iequale pal ion of1. >y the1 board" Standard Test Method for < . v Determination of the Decontaminabiiity of Coatings Used in Light-Water Nuclear Power Plants1 This standard is issued under the fixed designation D 4256; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last ceapproval. A superscript epsilon (' ) indicates an editorial change since the last revision or reapproval. ^1. Scope 3.1.3 disintegration of atomic nuclei--the nuclear trans 11.1 This test method establishes procedures for deter- formation characterized by the emission of one or more , rtinmg and ranking the ease ofdecontaminabiiity of coatings particles or photons from the nucleus. jjtfjp use in nuclear power plants. 3.1.4 disintegrations per minute (dpm)--the number of J .2 This standard defines two different test procedures disintegrations occurring in a time period of 1 min. ISplving differing contaminant contact times and deconjgjinating media. Procedure A involves a relatively brief 4. Significance and Use radionuclide solution contact time and decontamination 4.1' Day-to-day operation or a loss-of-coolant accident at a ' ^i;!'|hg both demineralized water and acid solutions. Proce- nuclear power plant can give rise to a significant level of " |e B utilizes a seven-day contamination solution contact radioactive contamination on the walls, floors, and attendant and decontamination with ambient temperature water equipment. The ease with which the coated surfaces can be Procedure B is more in line with power plant decon- decontaminated could result in considerable reduction in the ination practices. level of radioactive contamination, thereby mitigating the ;3 Users of this standard should specify either Procedure exposure to plant operating personnel. It is recognized that ir Procedure B, or both, based upon specific power plant this test method does not duplicate actual field decontami ditions and use requirements. nation procedures, but it does represent comparative test >4 This standard may involve hazardous materials, oper- procedures that have been in use for many years. Other tests, ms, and equipment. This standard does not purport to designed to be more meaningful in terms of real-life condi tyess all ofthe safety problems associated with its use. It is tions, are under development. responsibility of the user of this standard to establish 'opriate safety and health practices and determine the 5. Apparatus Wicability ofregulatory limitations prior to use. 5.1 Radiation Detection Equipment5--Use a gamma-sen sitive system composed of the following items: Referenced Documents 5.1.1 Detector--Use a germanium crystal detector with a l|l ASTM Standards: >.1193 Specification for Reagent Water2 resolution of 2.5 keV at 1332 keV or better. N' --See Method' E 522ifor calibration methods. p-522 Method of Calibrating Germanium Detectors for 5.1.2 Photomultiplier-Amplifier:6 ; Measurement of Gamma-Ray Emission Rates of Ra 5.1.3 Analog-to-Digital Converter (ADC).1 dionuclides3 5A A Pulse-Height Analyzer, capable of resolving simple |2 American National Standards Instituted gamma-ray peaks shall be used. 1512 Protective Coatings (Paint) for the Nuclear Industry 5.2 Mount test specimens so as to give an optimum scanning geometry of the contaminated surface. Terminology 5.3 Shield the detector to eliminate excessive background ,1 Definitions: counts. 3.1.1 decontaminate--the removal of radionuclides from st panel using prescribed procedures. f.il.2 decontamination factor {DP)--the ratio of the origkl radioactivity (dpm) to the radioactivity detected after Itment. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem- IjThis test method is under the jurisdiction of ASTM Committee D-33 on ictivc Coating and Lining Work for Power Generating Facilities and is the !&i responsibility of Subcommittee D33.U on Decontamination of Coated Faces. Current edition approved Feb. 24, 1989. Published June 1989. Originally " Jied as D 4256 - 83. Last previous edition D 4256 - 83. ^Annual Book ofASTM Standards, Vols 06,03 and II.01. ^Discontinued--see 1983 Annual Book ofASTM Standards, Vol 12.02. ` Available from American National Standards Institute, 11 W. 42nd St., 13th ir, New York, NY 10036. 5 The most up-to-date information on gamma-ray detectors and accompanying electronics is found in manufacturers' literature. A list of vendors of this equipment can be found in compilations such as the Guide to Scientific Instruments, published by the American Association for the Advancement of Science, Washington, DC. 6Tennelec Model TC-205, or equivalent, has been found satisfactory for this purpose. 7 Nuclear Data Model ND570, or equivalent, has been found satisfactory for this purpose, 699 DU PO50297881 D4256 ical Society, where such specifications are available.8 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean Type II reagent grade water conforming to Specification D 1193. 6.3 Contaminating Solution: 6.3.1 Use a radioactive contaminant solution of mixed fission products of cobalt-60 and cesium-137, prepared in 8 M nitric acid (HN03) and stored in a polyethylene bottle. 6.3.2 The solution shall have a minimum beta-gamma activity of 5 x 10* disintegrations per minute (dpm) per 0.1 mL. 6.4 Decontaminating Solutions--The following decon taminating solutions shall be utilized, based upon the proce dure selected (Procedure A or Procedure B): 6.4.1 An aqueous mixture of 0.4 M oxalic acid (COOH)2, 0.05 M sodium fluoride (NaF), and 0.3 M hydrogen peroxide <H202). 6.4.2 Demineralized water. Test Specimen A (Frontl 7. Preparation of Test Specimens 7.1 Steel Panels--Prepare panels in accordance with ANSI N5I2. 7.2 Concrete Blocks--Prepare blocks in accordance with ANSI N512. 8. Test Specimens 8.1 Use a minimum of two test specimens for each coaling system. 9. Specimen Contamination 9.1 Degrease the test specimens using the coating manu facturer's approved solvent; place on a level surface inside a laboratory hood and at 24 3C until the solvent has evaporated. Maintain a minimum air velocity of 150 ft/min at the face of the hood. 9.2 Transfer a portion of the contaminating solution to a clean polyethylene bottle and immediately adjust to pH 4 with 8 M ammonium hydroxide (NaOH). 9.3 Contamination Procedure A, Evaporate to Dryness: 9.3.1 Immediately transfer a 0.2-mL portion of the pHadjusted solution to the center of the lower 2-in. section of the test specimen so as to cover an area about 1 cm in diameter. 9.3.2 Allow the specimen to air dry as in 9.1, and place it in a plastic bag approximately 1.5-mil thick. 9.3.3 Position the specimen and bag in the detector chamber and scan, using identical geometry as in 8.2. Record all counts. 9.4 Contamination Procedure B, Seven-Day Contact Time: 9.4.1 Perform contamination using the assembly shown in Fig. 1. "Reagent Chemicals, American Chemical Society Specifications,'' Am. Ghentical Soc.. Washington. DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin. D. Van Nostrand Co.. Inc., New York, NY, and the "United States Pharmacopeia." FIG. 1 Top View of Holder for Contamination of Test Specimen in Seven-Day Exposure (Procedure B) 9.4.2 A test specimen is pushed into the positioning aid with its reference corner R as shown in Fig. 2. Edges A andB ofthe test specimen are brought into close contact with Lii s a and b of the positioning aid, the Contact B-b having priority. The test .specimen is then pressed against Part ' containing the silicone rubber ring by fastening the sere1. until the test specimen is in contact with Part V along all op us edges. 9.4.3 The test specimens are contaminated by applying i mL of the contaminant solution to the middle of the circle visible through Part f/.tThe holder shall be kept ill a horizontal position. If, in the case of highly hydrophobic surface materials, the contaminant does not immediately cover ihe test circle, the holder may be tilted to enforce sufficient spread of the liquid. 9.4.4 A small petri dish is placed over the test circle on t of Part U to prevent evaporation of the contaminant solution. 9.4.5 After seven-days contact time the contaminant solu tion is sucked offas completely as possible using a pipet. For this purpose it is necessary to tilt the holder. The holder is , then inverted. After removing the nuts and Part L, lift the test specimen vertically so that distribution of contaminant solution to uncontaminated parts of the test specimen is prevented. 9.4.6 To avoid evaporation effects immediately place the test specimen in a plastic bag. The whole procedure of removing the specimens from their holders and packaging them shall not take more than 12 min. 9.4.7 Position the contaminated specimens and scan as in 9.3.3. 10. Decontamination Procedure 10.1 The decontamination process for Procedure A will 700 DU P050297882 Contain itiation from this side FIG. 2 Cross Section of Holder for Contamination in Seven-Day Exposure (Procedure B) ,i jfcorporate ambient water (10.2), ambient acid (10.3), and lot add (10.4). The decontamination process for Procedure Hi?will incorporate only ambient water (10.2). ; 10.2 Decontamination With Water: 10.2.1 Place a 600-mL polyethylene beaker containing 4do mL of demineralized water (24 3"C) and a plastictbvered stirring bar on a magnetic stirrer. 10.2.2 Rigidly suspend the sample in the water to a depth tjof 2 in. with the contaminated side facing the center of the tbeaker. 10.2.3 Adjust the speed of the stirrer until the water J '.ortex touches the stirring bar; stir for 10 min. 1 10.2.4 Remove the sample, rinse the back (uncon taminated side) with water, and air dry the contaminated face as in 9.1. 10.2.5 After the sample has dried, transfer it to a clean plastic bag and scan as before. 10.2.6 The ratio of the original radioactivity (counts per minute) to the radioactivity detected after the water wash is recorded as the decontamination factor (DF) for the water wash. 10.3 Decontamination With Ambient Acid: 10.3.1 Using the same sample as for 10.2, perform a second decontamination as described in 10.2, except use the acid solution described in 6.4.1 at a temperature of 24 3C. 10.3.2 The ratio of radioactivity after the water wash to radioactivity after the acid wash is recorded as the DF for the cold acid wash. 10.4 Decontamination With Hot Acid: 10.4.1 Continuing to use the same sample as in 10.3, perform a third decontamination as described in 10.3, except heat the acid to 80 3C. 10.4.2 The ratio of radioactivity after the cold acid wash to radioactivity after the hot acid wash is recorded as the DF for the hot add wash. 10.5 The ratio of radioactivity before the water wash to radioactivity after the hot acid wash, with a possible correc- 701 DU P0502 97883 D 4256 A tion for natural radioactive decay described in 11.1, is recorded as the overall DF. 10.6 Control Sample: 10.6.1 Scan a contaminated, untreated control sample at the time the original and final counts are made on the test specimen. 10.6.2 Record any decrease in radioactivity. 10.6.3 Add this decrease to the value for the radioactivity after the final wash to calculate a corrected DF. The final wash will be with hot acid for Procedure A and with water for Procedure B. 11. Calculation 11.1 Calculate the decontamination factor (DF) (in con sistent units) as follows: j3P _ original activity activity after treatment 11.2 Calculate percent removed as follows: % removed 12. Report 12.1 The report shall include the following: 12.1.1 Procedures and conditions relating to the test specimen preparation, 12.1.2 Decontamination factors for each procedure, 12.1.3 Percent activity removed for each procedure, and 12.1.4 Any deterioration of the coating due to the test procedure. 13. Testing Laboratory 13.1 Testing shall be conducted by an independent testing laboratory. This laboratory shall not be affiliated in any manner with the coating manufacturer without the prior approval of the purchaser. 13.2 The testing laboratory shall be responsible for the documentation, reporting, and certification of all test results, 13.3 The testing laboratory shall be responsible for meeting the quality assurance requirements of the owner. _ original activity - activity after decontamination original activity x iOO too 14. Precision and Bias 14.1 The overall precision and bias of this test method have not been established. The American Society tor Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of suoh rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.r Philadelphia, PA 19103. 702 DUP0502 97884 T Last ASTM Designation: D 4257 - 87 test and test ting any 'it >1 the tits. ; foi Standard Practice for Design and Use of Safety Alert System for Hazardous Work Locations in the Coatings and Lining Industry * 7 bis practice covers a safety alert system for hazardous work locations and materials for the coatings and lining application ` istry. This practice is designed for multi-employer work sites. I jrmerly under the jurisdiction of Committee D-33 on Protective Coatings and Lining Work for Power Generation fifties, this practice was discontinued in 1989. I <1,1 703 DU P050297885 Designation: D 4258 - 83 {Reapproved 1988) Standard Practice for Surface Cleaning Concrete for Coating1 This standard is issued under the fixed designation D 4258; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice includes surface cleaning of concrete to remove grease, dirt, and loose material prior to the applica tion of coatings. Procedures include broom cleaning, vacuum cleaning, air blast cleaning, water cleaning, deter gent water cleaning, and steam cleaning. 1.2 This practice is not intended to alter the surface profile of the concrete but to clean the surface. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 5. 2. Referenced Documents 2.1 ASTM Standards: D4259 Practice for Abrading Concrete2 D4260 Practice for Acid Etching Concrete2 D4262 Test Method for pH of Chemically Cleaned or Etched Concrete Surfaces2 D4263 Test Method for Indicating Moisture in Concrete by the Plastic Sheet Method2 D4285 Test Method for Indicating Oil or Water in Compressed Air2 2.2 Other Standard: ACI-308 Recommended Practice for Curing Concrete3 3. Summary of Practice 3.1 Surface cleaning is intended to provide a clean, contamination-free surface without removing concrete from intact, sound surfaces. 3.2 Acceptable surfaces shall be free of oil, grease, loosely adhering concrete, and other contamination. Fins and pro jections shall be corrected prior to surface cleaning. 3.3 Air, water cleaning, scrubbing, sweeping, or vacu uming are acceptable cleaning methods. Cleaning agents may also be used to remove oil and grease spots followed by a fresh water rinse. 3.4 Any one or a combination of the listed cleaning procedures may be used to achieve acceptably cleaned 1 This practice is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work far Power Generating Facilities and is the direct responsibility of Subcommittee D33.05 on Surface Preparation. Current edition approved June 24, 1983. Published November 1983. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Available from American Concrete Institute, 22400 W. Seven Mile Rd., Detroit, MI 48219. surfaces. 4. Significance and Use 4.1 Surface cleaning is used to prepare concrete surface, for applying coatings intended for light-duty service, 4.2 Use of this practice alone is not intended when protective systems will be used for continuous or intermit tent immersion, mechanical loading, or for protective sys tems needing optimum bond for satisfactory performano (see Practices D 4259 and D 4260). 5. Cautions 5.1 New concrete shall be cured according to ACI-308 and sufficient additional time allowed for drying. 5.2 Moisture in the concrete may be detrimental to coating adhesion. Moisture content shall be in compliance with coating manufacturer's recommendation (see Tes Method D 4263). 5.3 Concrete cure compounds, form release materials, or concrete hardeners not compatible with the coating ma> require removal by other surface preparation methods as in Practice D 4259. 6. Procedures 6.1 Broom Cleaning: 6.1.1 This procedure is intended to remove most surface dust and other loosely adherent solid contaminants. 6.1.2 Broom cleaning shall consist of sweeping the surfao with a clean industrial stiff-bristled broom or similar device Sweepings shall be removed from the immediate work area 6.1.3 Broom-cleaned surfaces require additional cleaning using one or more of the surface preparation procedures specified in 6.2 through 6,6. 6.2 Vacuum Cleaning: 6.2.1 This cleaning procedure is intended to removi surface dust and other debris. 6.2.2 Vacuum cleaning shall consist of vacuuming th< surface with a heavy-duty type industrial vacuum to provid; an essentially dust-free surface. 6.3 Air Blast Cleaning: 6.3.1 This procedure is intended to remove debris, dust, dirt, loosely adherent laitance, and concrete from walls ant ceilings and to provide an essentially sound dust-free surface 6.3.2 Air blast cleaning shall consist of cleaning the surface with a compressed air stream at 80 to 100 psi through a blasting nozzle held approximately 2 ft from the surface. 6.3.3 The air stream shall be free of oil. This may bi verified using Test Method D 4285. 6.3.4 Surface cleanliness is dependent upon carrying off air-borne dust before it is redeposited. Vacuum cleaning ma; be required to remove redeposited dust. 704 3,1 DUP050297886 Water Cleaning: .1 This procedure is intended to remove dust, dirt, and soluble surface contaminants. j|.2 Water cleaning shall consist of cleaning the surface U stream of clean potable water having sufficient jure to remove dust, dirt, and loose material. When sarv, hand scrub with a stiff-bristled brush. 1.3 Prior to water cleaning, provisions shall be made for moval of wash water and contaminants generated by cleaning method. 1.4 The cleaned surface may be tested for moisture nt in accordance with Test Method D 4263 prior to " 'ng coatings. 5 Detergent Water Cleaning: 5.1 This procedure is intended to remove water-soluble e contaminants and oils, grease, and other emulsifiable 'als on the surface. 5.2 Detergent water cleaning shall consist of scraping off vy deposits of grease or oil and cleaning the surface with tiff-bristled biush using an aqueous solution of detergent Onsolvent emulsifier. Immediately after treatment, bethe surface dries, residues of the cleaning agent shall be ved by thoroughly flushing the surface with clean le water. Repeat flushing until the pH of the surface 'i meets the acceptance criteria of Test Method D 4262. 5.3 Trisodium phosphate at not less than 4 oz/gal, or iprietary products intended for cleaning concrete, may be S following manufacturers instructions. The effectiveness trisodium phosphate may be improved with the use ofhot or. 0.5.4 Repeat 6.5.2 until water does not bead on the aces. o T5 Prior to detergent water washing, provisions shall be dc for the removal of wash water and contaminants nerated by this cleaning method. 6.5.6 The cleaned surface may be tested for moisture content in accordance with Test Method D 4263. 6.6 Steam Cleaning: 6.6.1 This cleaning procedure is similar to detergent water washing, but is more effective for the removal of heavy deposits of grease and oil. 6.6.2 Steam cleaning shall consist of cleaning the surface with a jet of high-pressure steam sufficient to remove contaminants. 6.6.3 Detergents or nonsolvent emulsifying agents in tended for use with steam cleaning equipment may be added where required for removal of oil and grease. 6.6.4 When detergents or other emulsifying agents are used, after cleaning and before the surface dries, the surface shall be thoroughly flushed with potable water. Repeat flushing may be necessary to remove cleaning residues. 6.6.5 The surfaces cleaned with detergent or nonsolvent emulsifying agents shall be tested for pH in accordance with Test Method D 4262 and may be tested for moisture content in accordance with Test Method D 4263 prior to applying coatings. 6.6.6 Prior to steam cleaning, provisions shall be made for the removal of water and contaminants generated by this cleaning method. 7. Inspection 7.1 Visually examine the prepared surface for the pres ence of debris, dust, dirt, oil, grease, loosely adherent concrete, and other contaminants. 7.2 Test surfaces cleaned with detergent or nonsolvent emulsifying agents for pH following Test Method D 4262. 7.3 Moisture content may be determined following Test Method D 4263. 8. Acceptance 8.1 Acceptable surfaces shall be free of oil, grease, loosely adhering concrete, and other contamination. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determinationiof the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 705 DUPO 50297887 (Jjj p Designation: D 4259 - 88 Standard Practice for Abrading Concrete1 This standard is issued under the fixed designation D 4259; the number immediately following the.designation indicates the year of original adoption or, in the-case of revision, the year of last revision. A number in parentheses indicates the yearoflast reapproval. A superscript epsilon (r) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice includes surface preparation of concrete to prepare the surface prior to the application of coatings. 1.2 This practice is intended to alter the surface profile of the concrete and to remove foreign materials and weak surface laitance. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 5. 2. Referenced Documents 2.1 ASTM Standards: D4258 Practice for Surface Cleaning Concrete for Coating2 D4263 Test Method for Indicating Moisture in Concrete by the Plastic Sheet Method2 D4285 Test Method for Indicating Oil or Water in Compressed Air2 D4541 Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers2 2.2 Other Standard: ACI-308 Recommended Practice for Curing Concrete3 3. Summary of Practice 3.1 This practice is intended to provide a clean, contami nation-free, and roughened surface. 3.2 Acceptable surfaces shall be free of laitance, form release agents, curing agents, oil, grease, and other pene trating contaminants. The surface shall be free of fins, projections and loosely adhering concrete, dirt, and dust particles. 3.3 For some applications, a minimum concrete surface strength may he required for proper coating performance. 3.4 Acceptable methods of preparation include abrasive blasting (wet or dry), mechanical abrading, water blasting, and other similar procedures that will alter the surface profile of the concrete. 1 This practice is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities and is the direct responsibility of Subcommittee D33.05 on Surface Preparation. Current edition approved Feb. 26, 1988. Published April 1988. Originally published as D 4259 - 83. Last previous edition D 4259 - 83. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Available from American Concrete Institute. 22400 W. Seven Mile Rd., Detroit, MI 48219. 4. Significance and Use 4.1 This practice is used to prepare concrete for coating, where optimum bond is desired for service conditions such as continuous or intermittent immersion, temperature cy cling, or mechanical loading. 5. Cautions 5.1 New concrete shall be cured in accordance with ACI-308. 6. Mechanical Abrading Procedure 6.1 Suitable Surfaces--Mechanical abrading is suitable, for use on formed surfaces and floors and for the removal m fins and projections. 6.2 Pre-Surface Preparation: 6.2.1 Remove grease, oil, and other penetrating contami nants, (See Practice D 4258.) 6.2.2 Concrete surfaces may be wet or dry as appropriate to the type of equipment to be used. 6.3 Apparatus: 6.3.1 Typical apparatus covered by this method are rotai impact, vertical impact, and circular grinding equipment, i 6.3.2 Use the equipment in accordance with the manufae- ] turer's instructions in an organized manner in order fa thoroughly cover the entire surface to be prepared. 6.4 Appearance ofPrepaid Surface: 6.4.1 The intent is to remove sufficient material in order to achieve a sound concrete surface free of laitance, glazi efflorescence and incompatible concrete curing compounds or form release agents. 6.4.2 The surface shall have a roughened, textured ap-j pearance. Aggregate may be exposed. A roughness standard j may be established by mutual agreement. 6.4.3 The appearance will vary depending upon the. equipment used and type of concrete. 6.5 Post-Surface Preparation Cleaning--Clean in accord ance with Practice D 4258 to remove loose material. 7. Water Blast Cleaning 7.1 Suitable Surfaces--This method is suitable for use on formed surfaces and floors. 7.2 Pre-Surface Preparation: 7.2.1 Remove grease, oil, and other penetrating contami nants (see Practice D 4258). 7.2.2 Correct fins and protruding irregularities by me chanical means. 7.2.3 Concrete surface may be wet or dry. iliiM '4a' peej feeI 8. J *'8.i .*>S! P8.| Itofl R'T Is S,* ` ,* : * -T \hcc m A' * a jjjpi, r 706 DUP050297888 7.3 Apparatus--Typical apparatus covered by this hod is a piston-type positive displacement pump, highsure water blasting unit. The cleaning medium shall be ble water. Appearance ofPrepared Surface: ,4.1 The prepared surface shall be clean and free of dust, ': laitance and efflorescence. 1.2 The surface shall have a roughened textured appearA roughness standard may be established by mutual cement. $ Post-Surface Preparation Cleaning--Clean in accord s' with Practice D 4258 to remove loose material. |brasive Blast Cleaning Procedure Pre-Surface Preparation: 1)1.1 Remove grease, oil, and other penetrating contami- ; (see Practice D 4258). 1.2 Correct fins and protruding irregularities by mecal means. :.3 Concrete surface may be wet or dry as appropriate i type of equipment to be used. Suitable Surfaces--This method is suitable for use on Jjd surfaces and floors. J Apparatus: .l Typical methods are wet or dry open-blast cleaning fnozzles and self-contained recirculating blast-cleaning atus. i|2 The air stream used for nozzle blast cleaning shall be "f oil. This may be verified using Test Method D 4285. 'f.3 Use the equipment in accordance with the manufac-, fis instructions. s Appearance ofPrepared Surface: 8.4.1 The intent is to remove sufficient material in order to achieve a sound concrete surface free of laitance, glaze, efflorescence, and incompatible concrete curing compounds or form release agents. 8.4.2 The surface shall have a roughened textured appear ance. A roughness standard may be established by mutual agreement. 8.4.3 Some aggregate may be exposed and bug holes shall be opened. 8.5 Post-Preparation Cleaning--Clean in accordance with Practice D 4258 to remove loose material. 9. Inspection 9.1 Visually examine the prepared surface for loose ad hering concrete, thin crusts bridging voids, fins, and projec tions. 9.2 Visually examine the prepared surface for oil, grease, and markings. 9.3 If required, surface strength may be determined in accordance with Method D4541 or other agreed upon method. 10. Acceptance 10.1 Acceptable surfaces shall be free of laitance, oil, grease, and other materials incompatible with the coating. The surface shall also be free of fins, projections and loosely adhering concrete, dirt, and dust particles. 10.2 The surface shall have a roughened, textured appear ance. Aggregate may be exposed. Bug holes shall be opened. 10.3 The roughened textured appearance shall be similar to the roughness standard established by mutual agreement. 10.4 If specified, the treated surface shall meet the surface strength requirements. The American Society for Testing and Materials takes no position respecting the validity of any patent rights assortedin connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. DUP050297889 Designation: D 4260 - 88 ;/w. A Standard Practice for Acid Etching Concrete1 This standard is issued under the fixed designation D 4260; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope LI This practice includes surface preparation of concrete to prepare the surface prior to the application of coatings. 1.2 This practice is intended to alter the surface profile of the concrete and to remove foreign materials and weak surface laitance. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 5. 2. Referenced Documents 2.1 ASTM Standards: D4258 Practice for Surface Cleaning Concrete for Coating2 D 4259 Practice for Abrading Concrete2 D4262 Test Method for pH of Chemically Cleaned or Etched Concrete Surfaces2 D4263 Test Method for Indicating Moisture in Concrete by the Plastic Sheet Method2 D4541 Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers2 2.2 Other Standard: ACI-308 Recommended Practice for Curing Concrete3 3. Summary of Practice 3.1 This practice is intended to provide a clean, contami nation-free, and roughened surface. 3.2 Acceptable surfaces shall be free of laitance, form release agents, curing agents, oil, grease, and other pene trating contaminants. The surface shall be free of fins, projections, and loosely adhering concrete, dirt, and dust particles. 3.3 For some applications, a minimum concrete surface strength may be required for proper coating performance. 4. Significance and Use 4.1 This practice is used to prepare concrete for coatings where optimum bond is desired for service conditions such 1 This practice is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities and is the direct responsibility of Subcommittee D33.05 on Surface Preparation. Current edition approved Feb. 26. 1988. Published April 1988. Originally published as D 4260 - 83. Last previous edition D4260 - 83. 2 Annua! Book ofASTM Standards, Vol 06.(11. 3 Available from American Concrete Institute, 22400 W. Seven Mile Rd,, Detroit, MI 48219. as continuous or intermittent immersion, temperature cy cling, or mechanical loading. 5. Cautions 5.1 New concrete shall be cured in accordance with ACI-308. 5.2 Concrete cure compounds, form release materials, or: concrete hardeners may require abrading, in accordance with Practice D 4259, as acid etching may not be effective. 5.3 All oil and grease shall be removed in accordance with ' Practice D 4258 prior to mechanical abrading, abrasive blast cleaning, water blasting, or acid etching. 5.4 Use and disposal of materials should conform to established federal, state, local, and project requirements. 6. Acid Etching Procedure 6.1 Pre-Surface Preparation: 6.1.1 Remove grease, oil, and other penetrating contami nants (see Practice D 425 8). 6.1.2 Remove fins and protruding surface irregularities by mechanical means. 6.1.3 Surfaces shall be free of standing water. 6.1.4 Some curing compounds may not be removed by acid etching and will require preparation by mechanical abrading, abrasive blasting, or water blasting in accordance, with Practice D 4259. 6.2 Suitable Surfaces: 6.2.1 This method is primarily suited for use on hori zontal surfaces. 6.2.2 Other methods of preparation may be more suitable i, for rough concrete surfaces and walls or overhead surfaces. 6.3 Acid Etching Solutions: 6.3.1 Typical solutions covered by this method arc muriatic (hydrochloric), sulfamic, phosphoric and citnc acids. Hydrochloric acid shall not be used where chlorid are prohibited. 6.3.2 The acid concentrations of etching solutions may , vary, depending on the concrete texture and degree of' etching required. 6.3.3 The concrete surface shall be pre-wet with water prior to applying etching solutions. Free-standing water shall be removed. Uniformly apply the etching solution to the wet surface. Polyethylene sprinkling cans are suitable for ap plying acid solutions. Bubbling should be uniformly evident. If not, this indicates the presence of grease or oil contaminrtion, or both, curing compounds or sealers, or a need to increase the concentration of the acid solution. Scrub the acid wetted surface with a stiff bristle brush. 6.3.4 When the etching solution bubbling begins to sul side, flush surfaces to remove reaction products, and inspei; for uniform roughening and removal of laitance. Repea 708 DUP050297890 a* 04260 application of acid to obtain required surface. * fi.3.5 After the desired roughening is achieved, thoroughly jjjffjsh the surface with potable water. Repeated flushing and 7Stubbing with a stiff-bristled brush may be necessary to /remove acid residues. jrjJf j.3.6 The acid etched surface shall be tested for pH in a. jordance with Test Method D 4262 and may be tested for isture content in accordance with Test Method D 4263 I" j.or to applying coating. 6. ^ Appearance ofPrepared Surface: " 6.4.1 The intent is to remove sufficient material in order igp achieve a sound concrete surface free of laitance, glaze, R[florescence, and incompatible concrete curing compounds form release agents. ' r 6.4.2 The acid etched surface shall be uniformly rough ened to a degree similar in appearance to a medium to coarse 'f. grade sandpaper. A roughness standard may be established i'1" !> . mutual agreement. I-Inspection k '.1 Visually examine the prepared surface for loose ad hering concrete, thin crusts bridging voids, fins, and projec tions. 7.2 Visually examine the prepared surface for oil, grease, and markings. 7.3 Test surfaces cleaned by acid etching for pH in accordance with Test Method D 4263. 7.4 If required, surface strength may be determined in accordance with Method D4541 or other agreed upon method. S. Acceptance 8.1 Acceptable surfaces shall be free of laitance, oil, grease, and other, materials incompatible with the coating. The surface shall also be free of fins, projections, and loosely adhering concrete, dirt, and dust particles. ' 8.2 The surface shall have a roughened, textured appear ance. Aggregate may be exposed. Bug holes shall be opened. 8.3 A roughness standard may be established by mutual agreement. 8.4 If specified, the treated surface shall meet the surface strength requirements. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection in with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, wd the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Yourcomments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical commutee,' which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Rade St., Philadelphia. PA 19103. . St ?; If I* 709 DUP0502 97891 Designation: D4261 - 83 (Reapproved 1988) Standard Practice for Surface Cleaning Concrete Unit Masonry for Coating1 This standard is issued under the fixed designation D4261; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or rcapproval. 1. Scope 1.1 This practice covers surface cleaning of concrete unit masonry to remove dust, dirt, mortar spatter, oil, and grease prior to the application of coatings. Procedures include vacuum cleaning, air-blast cleaning, water cleaning, deter gent water wash, steam cleaning, and mechanical cleaning. 1.2 This practice is not intended to alter the surface profile'ofthe concrete masonry units but to clean the surface. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safetyproblems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 5. 2. Referenced Documents 2.1 ASTM Standards: D4258 Practice for Surface Cleaning Concrete for Coating2 D4262 Test Method for pH of Chemically Cleaned or Etched Concrete Surfaces2 D4263 Test Method for Indicating Moisture in Concrete by the Plastic Sheet Method2 2.2 Other Standard: ACI Specification 531.7-76 Specification for Concrete Masonry Construction3 3. Summary of Practice 3.1 Surface cleaning is intended to provide a clean, contamination-free surface suitable for the application of coatings. 3.2 Acceptable surfaces shall be free of dust, dirt, mortar spatter, oil, grease, and other contaminants. Mortar joints shall be struck flush or tooled with a round jointer and shall be free of rough edges and nibs (see ACI 531.1-76). 3.3 Vacuum cleaning, air blast cleaning, water cleaning, detergent water wash, steam cleaning, hand tool, and me chanical cleaning are acceptable cleaning methods. 1 This practice is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities and is the direct responsibility of Subcommittee D33.05 on Surface Preparation. Current edition approved Aug, 17, 1983. Published November 1983. 2 Annua/ Book ofASTM Standards, Vo! 06.0J. 'Available from American Concrete Institute, 22400 W. Seven Mile Rd., Detroit, MI 48219. 3.4 Any one or a combination of listed cleaning proce dures may be used to achieve acceptably cleaned surfaces. 4. Significance and Use 4.1 Surface cleaning is to be used to prepare concrete unit masonry surfaces for applying coatings intended for light duty service, splash and spillage of water and chemical* solutions, radiation exposure, decontamination, and re peated washdowns with alkaline cleaners. 5. Cautions 5.1 Moisture in concrete unit masonry may be demmental to coating adhesion. Moisture content shall be in compliance with the coating manufacturer's recommenda tions (see Test Method D4263 for moisture test method), 6.. Procedures 6.1 Steam Cleaning--This procedure is intended to re move heavy deposits of grease and oil, as well as other water soluble surface contaminants and emulsifiable materials, with a jet of high pressure steam, in accordance with Practice D 4258. 6.2 Detergent Water Wash--This procedure is intended to remove water soluble surface contaminants, oils, grease, and other emulsifiable materials with an aqueous solution of detergent or nonsolvent emulsifier in accordance with Prac tice D 4258. 6.3 Water Cleaning--^This procedure is intended to move dust, dirt, and water soluble contaminants with a stream of water under pressure, in accordance with Practice,, 4 D 4258. 6.4 Mechanical Tool Cleaning: 6.4.1 The intent of this procedure is to remove mortar1 2 spatter, efflorescence, and similar dry, firmly adhering for eign material prior to performing either cleaning operation. > 6.4.2 This procedure shall consist of scraping, abrading, brushing, or stoning to dislodge mortar and similar materials from the surface. 6.4.3 Clean in accordance with Practice D 4258 to re move dust and loose particles. 6.5 Vacuum Cleaning--This procedure is intended remove surface dust and other debris by vacuum cleaning in accordance with Practice D4258. 6.6 Air Blast Cleaning--This procedure is intended ti remove debris, dust, dirt, and loosely adhering material b: air blast cleaning in accordance with Practice D 4258. 7. Inspection 7.! Visually examine prepared surface for the presence ol debris, dust, dirt, oil, grease, loose particles, mortar spatter, and other contaminants. 710 DUPO 50297892 D 4261 7.2 Test surfaces cleaned with detergent or non-solvent ilsifying agents for pH in accordance with Test Method )4262. 7.3 Moisture content may be determined in accordance with Test Method D 4263. 8. Acceptance 8.1 Acceptable surfaces shall be free of dust, dirt, mortar spatter, oil, grease, and other contaminants. cc:s The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a (air hearing you should make your views known to the ASTM Committee on Standards, 1916 Race Si, Philadelphia, PA 19103. i-shi leal re- ;tri: in t. ida-. ` le tter ; d' ee::-!|1||'|* dedip ase, l.v Ttiiis re-j i al ica- 'tad cfcl* $8! tc^ ill , to' *ii*tfe 711 DUP050297893 Designation: D 4262 - 83 (Reapproved 1988) Standard Test Method for pH of Chemically Cleaned or Etched Concrete Surfaces1 This standard is issued under the fixed designation D 4262; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the procedure for determining the acidity or alkalinity of concrete surfaces prepared by chemical cleaning or etching prior to coatings. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Definition 2.1 pH--a measure of the hydrogen ion concentration and indicates whether a solution is acidic, alkaline, or neutral. 3. Significance and Use 3.1 Chemical cleaning or etching is used to prepare concrete for coating. 3.2 Residual chemicals not removed by water rinsing may adversely affect the performance and adhesion of coatings applied over prepared concrete surfaces. It is the intent of this test method to determine that residual chemicals have been removed by measuring the acidity or alkalinity of the final rinsed surface. 4. Apparatus 4.1 pH Test Paper, with a minimum range from 1 to 11 1 This test method is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities and is the direct responsibility of Subcommittee D33.05 on Surface Preparation. Current edition approved Aug. 17, 1983. Published November 1983. pH units with a capability of measuring in increments of 0.5 pH units. S. Materials 5.1 Potable Water, for rinsing chemically cleaned or etched concrete surfaces. 5.2 Wet Concrete Surface, following the final water rinsi and before the rinse water has completely drained off thi surface. V) I 6. Procedure 6.1 Tear off a strip of test paper, wet with test water and after the color develops, compare with color chart to determine pH. 6.2 The pH of the water used for rinsing shall be determined to establish acceptance criteria. Readings shall be taken at the beginning and end of the final rinse cycle. 6.3 At least two surface pH readings shall be taken for each 500 square feet or portion thereof. Readings shall be taken at randomly selected locations immediately following the final rinse and before all the rinse water has drained nit the surface. 6.4 Unless otherwise specified, tests shall be conducted inaccordance with this procedure. 7. Acceptance Criteria 7.1 The pH readings following the final rinse shall not more than 1.0 pH lower or 2.0 points higher than the pH of the rinse water (see 6.2) unless otherwise specified. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or foraddftional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel (rial your comments riave not received e fair hearing you sriou/d make your views known to the ASTM Committee on Standards. 1916 Race St., Philadelphia, PA 19103. 712 DUP050297894 Designation: D 4263 - 83 {Reapproved 1988)1 K _Jj|; * ** of 0.5 Standard Test Method for indicating Moisture in Concrete by the Plastic Sheet Methdd1 This standard is issued under the fixed designation D4263; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. N' --Editorial changes were made throughout in September 1988. ed or rinse ff the :r and irt to ill be fall be In foi all be owing edofl ted in lot be pH of Scope ,{.1 This test method is used to indicate the presence of pillary moisture in concrete. 1.2 This standard may involve hazardous materials, opermns, and equipment. This standard does not purport to itress all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish ipropriate safety and health practices and determine the tpiicabiUty of regulatory limitations prior to use. For dficcaution statements, see Section 4. Significance and Use It Capillary moisture in the concrete may be detrimental the performance of certain coating systems that cannot irate moisture on or within the surface boundary. 12 This test method is used prior to the application of atiags on concrete. Materials 3. 1 Transparent Polyethylene Sheet, commercially availslfy approximately 4 mils (0.1 mm)thick. :|2 Adhesive Tape that will adhere lo-the substrate.' (Duct : 2 in. (50 mm) wide is suggested.) Cautions fed This test method shall be conducted when the surface iffhis test method is under the jurisdiction of ASTM Committee D-33 on |biive Coating and Lining Work for Power Generating Facilities and is the | responsibility of Subcommittee D33.05 on Surface Preparation. |irrent edition approved Aug. 17. 1983. Published November t983. temperature and ambient conditions are within the estab lished parameters for application of the coating system. 4.2 Avoid direct sunlight, direct heat, or damage to the plastic sheet, as such treatment affects the reliability of the results. 5. Procedure 5.1 Tape a segment of plastic sheet, approximately 18 by 18 in. (457 by 457 mm), tightly to the concrete surface making sure that all edges are sealed. 5.2 Allow the plastic sheet to remain in place a minimum of 16 h. 5.3 After the allowed time has elapsed, remove the plastic sheet and visually inspect the underside of the sheet and the concrete surface of the patch for the presence of moisture. 5.4 Sampling: 5.4.1 Floors--One test area per 500 ft2 (46 m2) or portion thereof, of surface areas unless otherwise specified. 5.4.2 Walls and Ceilings--One test area per 500 ft2 (46 m2) or portion thereof, of surface area unless otherwise specified. 5.4.3 The recommended practice is a minimum of one test for each 10 ft (3 m) of vertical rise in all elevation starting within 12 in. (300 mm) of the floor. 6. Report 6.1 Report the presence or absence of moisture. 7. Precision and Bias 7.1 This test method indicates the presence of capillary moisture. No precision or bias has been established for this test method. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are express// advised that determination of the validity of any such patent rights, and the risk of infringement-of such rights, are entirely their own responsibility. V. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are fni/ited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 713 DUP050297895 (|jjjj|) Designation: D 4285 - S3 (Reapproved 1988) Standard Test Method for Indicating Oil or Water in Compressed Air1 This standard is issued under the fixed designation D 4285; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method is used to determine the presence of oil or water in compressed air used for abrasive blast cleaning, air blast cleaning, and coating application opera tions. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices knd determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 4. 2. Significance and Use 2.1 Clean compressed air is required to prevent contami nation of coating materials and surfaces being prepared for coating. This test method is a visual examination technique for determining oil or water in compressed air. Other types of contamination may require additional analytical techniques for detection. 3. Apparatus and Materials 3.1 Absorbent Collector, such as white absorbent paper or cloth and rigid backing for mounting absorbent collector, or 3.2 Nonabsorbent Collector, such as rigid transparent plastic, approximately Vs in. thick. 4. Cautions 4.1 To avoid false indications prior to testing: 1 This test method, is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generating Facilities and is the direct responsibility of Subcommittee 1333.05 on Surface Preparation. Current edition approved Sept. 30. 1983. Published December 1983. 4.1.1 Allow compressed air system to reach operatin' conditions, and 4.1.2 Allow air to discharge at operating conditions u, remove accumulated condensation in the system. 4.2 Fasten the collector material to the rigid backing, Avoid personal contact with the air stream. 5. Sampling 5.1 Conduct the test on discharging air as close to the use,,, point as possible and after the inline oil and water separators, > 6. Procedure 6.1 Use either the absorbent or nonabsorbent collector. - ,* 6.2 Position the collector within 24 in. ofthe air-dtscha gejp*l point, centered in the air stream. M 6.3 Adjust air discharge so that the collector remaias,g intact during the test Allow air to discharge onto theaf collector for a minimum of 1 min. jE 6.4 Visually examine the collector for the presence w, absence of oil or water, or both. 7. Interpretation of Results 7.1 Any indication of oil discoloration on the collector 3 shall be cause for rejection of the compressed air for use 11 abrasive blast cleaning, air blast cleaning, and coating^ application operations. 7.2 Any indications of water contamination on the cat lector shall be cause for rejection of the compressed air ftasfjj use in those applications where water is detrimental, such . s abrasive blast cleaning, air blast cleaning, and coating"^ application operations. 8. Precision and Bias 8.1 No precision or bias statement has been establish..! for this test method. The American Society lor Testing and Materials takas no position respecting the validity ol any patent rights asserted In connection with any Item mentioned In this standard. Users ol this standard are expressly advised that determination of the validity ol any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committBO and must be reviewed evory five years end If not revised, either reapproved or withdrawn. Your comments are Invited either lorrevision ol this standard or lor additional standards and should be addressed to ASTM Headquarters. Your comments will receive cerelut consideration at a meeting of the responsible technical committee, which you may attend. II you teeI that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 714 DU P050297896 Designation: D 4286 - 90 Standard Practice tor Determining Coating Contractor Qualifications for Nuclear Powered Electric Generation Facilities1 (Scope 1.1 This practice provides a criteria guide and procedural fethod to assist utility owners, architects, engineers, con- actors, and other selection agencies in determining the uirall qualifications of a coating contractor to execute ling work for the primary containment and other safetyated facilities of light-water nuclear power plants. 1.2 The qualification criteria and requirements address essential basic capability of a contractor to execute uclear coating work. Obviously, the specific capability to nfute those requirements unique to a given project must be carefully considered. The evaluation procedure gained in this practice is designed to be adaptive to this iled final qualification process. Variation or simplificai ofthe practice is appropriate for non safety-related areas ^'nuclear power plants, fossil fueled facilities, and other [stria! projects. 1.3 The overall capability of a contractor to successfully cgute the varied and complex requirements of nuclear ting work is dependent upon competency in a variety of Ihtial categories. j! The nine evaluation categories described in Sections 3 ough 12 detail the specific data to be provided by the Stractor as essential to determining qualification status. In fpition, a tenth untitled category has been provided on the '"filiation work described in Section 12 for inclusion of per information pertinent to a specific project. .5 This standard does not purport to address the safety bblems associated with its use. It is the responsibility ofthe of this standard to establish appropriate safety and %ahh practices and determine the applicability ofregulatory nations prior to use. Referenced Documents |l ASTM Standard: 13843 Practice for Quality Assurance for Protective ppoatings Applied to Nuclear Facilities2 ^ > 4537 Guide for Establishing Procedures to Qualify and P Certify Inspection Personnel for Coating Work in Nu clear Facilities2 2.2 American National Standard: 45.2.6 Qualifications of Inspection, Examination, and [ Testing Personnel for Nuclear Power Plants3 |3 Other Standard: `This practice is under the jurisdiction of ASTM Committee D-33 on ( active Coating and Lining Work for Power Generation Facilities and is the rtt responsibility of Subcommittee D33.07 on Application, urrent edition approved March 30, 1990. Published May 1990. Originally dished as D 4286 - 84. Last previous edition D 4286 - 84. f Annual Book ofASTM Standards, Vol 06.01. 5 Available from American National Standards Institute, 11 W. 42nd St., 13th sr, New York, NY 10036. Nuclear Regulatory Agency 10 CFR 50 Appendix B, Quality Assurance Criteria for Nuclear Power Plants4 3. Personnel 3.1 Home Office Management and Staff--Resumes of the following types of personnel including educational back ground, duration and degree of involvement in industrial coating operations, qualifications, registrations, certifica tions, and specific experience in nuclear coating work. 3.1.1 Principals and General Management. 3.1.2 Engineering Manager. 3.1.3 Project Engineers--List specific nuclear coating work project involvement. 3.1.4 QA/QC Manager--List specific qualification/cer tification credentials per ANSI N45.2.6, or Guide D 4537, or both. 3.2 General Field Supervision--Resumes to include spe cific nuclear coatings work experience. 3.3 On-Site Project Supervision: 3.3.1 Total number of personnel qualified for nuclear coatings work, including specific work history. 3.3.2 Total number available in a specific time frame, if appropriate. 4. Contractor Work Experience 4:1 General Experience--List of comparable industrial projects, including type (construction or maintenance), form of contract, dollar volume, scope, and duration (start and completion dates) executed during the past five years. Accompanying this listing provide personnel references to include names, titles, locations, and telephone numbers. 4.2 Nuclear Coating Work Experience: 4.2.1 List of nuclear projects including type (construction or maintenance), form ofcontract, dollar volume, scope, and duration, materials, and equipment involved. Accompa nying this listing provide personnel references to include names, titles, locations, and telephone numbers. 4.2.2 If the contractor has executed work comparable to the specific evaluation project, submit complete case histo ries of scope and functions performed to include personnel references for each case. 5. Equipment 5.1 List contractor-owned equipment in the categories listed in 5.1.1 through 5.1.9. Indicate those items required for the specific evaluation project. 5.1.1 Vehicles. 5.1.2 Surface preparation, all types. 5.1.3 Abrasive control and recovery. 5.1.4 Coatings mixing and application, all types. 4 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 715 k DUP050297897 ----- -- D 4286 5.1.5 Environmental control and curing. 5.1.6 Rigging and enclosure. 5.1.7 Safety. 5.1.8 Quality control testing instrumentation. 5.1.9 Specialized equipment. 5.1.9.1 Unique equipment required for the specific project, if applicable. 5.1.9.2 Contractor to indicate and provide examples of capability to design and install highly specialized items of equipment, enclosure systems, devices, etc. which have been utilized on previous nuclear coating projects. 5.1.10 Equipment Repair and Replacement Capability-- Contractor to describe standard procedure followed in the event of equipment failure to prevent lost time situations. 6. Quality Assurance 6.1 Quality Assurance Program--The contractor shall submit one copy of his quality assurance program that shall conform to 10 CFR 50 Appendix B, ANSI N 45.2.6, Guide D 4537, Practice D 3843, and other applicable documents. The program shall include implementation procedures and sample forms. 6.2 Quality Assurance/Quality Control--List number of personnel qualified in accordance with ANSI N 45.2.6 or Guide D 4537, or both, for each of the following: 6.2.1 LEVEL III Inspector, 6.2.2 LEVEL II Inspector, and 6.2.3 LEVEL I Inspector. 7. Training 7.1 Submit training manual for craft and supervisory personnel. If no formal training program exists, the con tractor shall submit evidence of procedures and methods utilized. 8. Safety 8.1 Submit copy ofcorporate safety program. If no formal program exists, the contractor shall submit evidence of safety procedures and work rules.9 9. Production/Cost Control 9.1 Submit explanation of methods and procedures uti lized to monitor and regulate personnel and equipment productivity. 9.2 Submit sample of actual report forms utilized to record job progress, labor cost analysis, and equipment deployment efficiency. 10. Financial 10.1 Submit documentation to verify financial capability to manage and execute all project requirements. Include the following data: 10.1.1 Current financial statement, 10.1.2 Trade references, three or more, 10.1.3 Bank references, one or more, 10.1.4 Bonding capacity, name of bonding company, and name and address of agent, and 10.1.5 Current certificate of insurance. 11. Current and Projected Performance Capability (re stricted to specific project considerations) 11.1 Submit a statement indicating current commitment status of personnel, equipment, and management capability. The statement shall include analysis of and ability to fulfill requirements in the following categories: 11.1.1 Craft personnel, 11.1.2 Staff engineering and supervisory personnel, 11.1.3 Management personnel, 11.1.4 Equipment, and 11.1.5 Materials. 12. Contractor Evaluation Work Sheet 12.1 The sample work sheet shown in Fig. 1 is suggested for consolidation of rating and comparison data. Note that there are nine basic rating categories corresponding to the criteria detailed in the text of this practice. Space for an optional tenth category has been provided for owner inser tion of other rating data that may be unique to the specific project involved. 12.2 Rating Values--Numerical rating values are struc tured on the following format: Rating Excellent Good Average Poor Unsatisfactory No data Value 4 .1 2 1 0 0 12.3 Weighted Category Values--Each of the ten (in- 1 eludes option) evaluation categories will be assigned fi| weighted value by the owner in accordance with the specilig|,, requirements of the project. The value scale will range from 1 (least critical) to 10 (most, critical). The weighted value of & each category will be used as a multiplier to determine the overall rating for each contractor in each category. 716 DUP050297898  D 4286 ReipraCapiatcy| [riTainng | L __ I_____ Evaluator: PERSONNEL (W.' IHome O ffic e | Sir.ractor "A" E I5 6 I i 3 EXPERIEKCE (W.V.- 1 fo If2P-fiIFNT (H.V.s ) 0 f) ,n r (w.v.* Title:_____ ) TR i iI I i ! i i i 1i 2 I II I I 2 1 s ii I I I 2I 1 ,o 3in I I I I 13 x Wmtor praetor "C" W>ctor "0" Ve- jfector "E" Sector "F" fecter "G'1 P/C CONTRO (W.V.= ) FINANCIAL (W.V.* 3 LIMITATIONS IW.V.s ) OPTION (U.V.* ) SUHMAFY rPocedrues | #J1ffeta,a'Cecmttoo,rr r|^Scrtfonrr "SV" """ECPr",*;] I 1 I i a I 1 I i I i1 2l I f I 1 i 3 I I1t ! 1 I J Z < !s j 1 Ia 1 I1 ~-- -- -- Rate Value: Excellent. * 4, Good * 3, Average * Z, Poor K Unsatisfactory = 0, Ho Data = 0. Weighted Value: l (Least Critical) through 10 (Most Critical) FIG. 1 Contractor Evaluation Work Sheet The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights,, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or lor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. II you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 717 DUP050297899 Designation: D 4287 - 88 Standard Test Method for High-Shear Viscosity Using the id Cone/Plate Viscometer1' This standard is issued under the fixed designation D 4287; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the viscosity ofpaints, varnishes, and related products at a rate .of shear of 12 000 s_I. > 1.2 Paints and varnishes that dry very rapidly may not give reproducible results with this test method. Measure ments made at elevated temperatures may also give poor precision due to loss of volatiles and to drying. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability or regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems12 3 D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 (0 to 1 Pa-s) or 0 to 5-P cone producing a rate of shear u 12 000 s~1. With higher viscosity materials, other cones (0 to 20 P, 0 to 40 P, 0 to 100 P) may be used on agreement between the producer and the user, but it should be notc_ that these give lower shear rates (~3000 s~`) not truly representative of application conditions. Other cone/plato viscometers may be used on agreement between the producer and the user as long as the same rate of shear is measured and it is approximately 12 000 s~'. However, results m, differ from those produced with an ICI cone/plate viscometer. N ' I--The SI units for viscosity are pascal-seconds (Pa-s, 1 P- , = 10 P, 1 mPa-s= t cP). 6. Reagents and Materials 6.1 Water or AWw/rt--Water or a low viscosity solventil such as xylene or mineral spirits to be used for zeroing th^J instrument. 6.2 Mineral Oils--Three standard mineral oils v,,ii known viscosities (certified by an approved laboratory) lying between 10 and 90 % or full scale.4 3. Summary of Test Method 3.1 The material to be tested is placed between the cone and plate of an 1C1 cone/plate viscometer, then subjected to a high shear rate while the viscosity is determined. 4. Significance and Use 4.1 The viscosity value obtained by this test method gives information about the flow properties of the material under application conditions: brushing, spraying, electrostatic disk, or roll coating. 4.2 This test method is suitable for all paints and var nishes whether they are Newtonian in behavior or not. However, due to the narrow gap between the stationary and rotary parts of high-shear viscometers, this test method is more reproducible for paints having finer pigment disper sions as determined by Test Method D 1210. 5. Apparatus 5.1 ICICone/Plate Viscometer3 (see Fig. 1) with 0 to 10-P 1 This lest method is under the jurisdiction or ASTM Committee D-l on Paint and Related Coalings and Materials and is the direct responsibility of Subcom mittee D01.24 on Physical Properties of Liquid Paints and Paint Materials. Current edition approved Oct. 31, f 988. Published December 1988. Originally published as D 4287 - 83. Last previous edition D 4287 - 83. 2 Annual Book ofASTM Standards, Vol 06.01. 3 ICI cone/plale viscometers are available from BYK.-Gardner, Inc.. Gardner Laboratory. 2435 Linden Lane, Silver Spring, MD 20910 and from Research Equipment (London) Ltd., 64 Wellington Rd., Hampton Hill, Middlesex TW12 IJX, England. 7. Sampling 7.1 Take a representative sample of the product to be tested in accordance with Practice D 3925. If the sample has a tendency to settle or separate on standing, it must be stirred or shaken until homogenepus before a test specimen is taken from it. The specimen must be free of any foreign matter or air bubbles and its volume must be sufficient to cover the portion of the viscometer plate under the cone when thai3j latter is brought into contact with the plate. 8. Preparation of Apparatus 8.1 Zero the apparatus daily when in regular use, or otherwise before use, by following the procedure in Section 9. but using a low viscosity liquid. If the pointer does not indicate zero, it may be adjusted by means of a lever on the left-hand side of the upper part of the instrument housing, if the instrument cannot be zeroed, it should be returned to the supplier for adjustment. 8.2 Verify the calibration of the apparatus by following the procedure in Section 9, but using standard refined mineral oils having Newtonian characteristics and known viscosities.4 If the viscometer pointer reads the correct viscosity (or within 5 % of that value) with two or more oils whose viscosities bracket those of specimens to be tested, then the viscometer readings may be used as is. If the 4 Such oils arc available from The Cannon Instrument Co., P.O. Box 16, Sta College, PA 16801. 718 DUP050297900 FIG. 1 ICI Cone/Plate Viscometer con leter readings do not give the correct viscosities for the then a calibration curve must be constructed by taking 1 iscometer readings for three oils and plotting measured |jsity versus specified (correct) viscosity for the oils. Jbquent measurements are corrected to true viscosities 8&h use of the curve. <`.3 Check the cones periodically for wear. Replace any i that shows a definite flattening of the apex. Some users found it necessary to replace cones every year. The determination must be made at a closely confed temperature of 25 0.3C unless otherwise agreed. In pr to check the temperature control, carry out the test as lifted in 9.1 with the standard refined mineral oil of the est viscosity. Allow the viscometer to run with this oil for pin and determine whether the reading decreases. If the -e is more than 10 %, the apparatus is unsuitable for ^determination of viscosities at high rates of shear in fedance with this test method. tore 2--Multitemperature ICI cone/plate viscometers have heating, ghot cooling, capabilities. Therefore, runs with these viscometers at ; should only be done at room temperatures at or below 22"C to tfe that the plate temperature does not go above 25C. The instruments that operate at 25"C only do have cooling capabilities and give better temperature control. 9. Procedure 9.1 With the cone in the down position, turn the instru ment on and allow it to warm up for at least 5 min. For a multitemperature instrument, set the dial at 25C or to an alternatively agreed upon temperature. Raise the cone to the up position. Transfer a suitable amount of the product to be tested to the plate, taking care to avoid the inclusion of air bubbles, and'again lower the cone to the down position. Wait for 30 s to allow the specimen to attain the agreed upon temperature. 9.2 Start the cone rotating and record the reading on the scale (Note 3) when the pointer becomes steady. Non- 3--Whether the. reading gives a direct indication of the viscosity or not, depends on the cone and scale used. N' 4--In some cases it is difficult to judge whether a constant reading has been obtained. However, if the pointer does not become steady after 15 s, record the reading at 15 s and mention the lack of a constant reading in the test report. If highly accurate readings are required, make the readings below 90 % of the scale. 9.3 If the reading does not directly indicate the viscosity, multiply the reading by the appropriate conversion factor or use the appropriate calibration curve to obtain the viscosity. 9.4 Clean both the cone and the plate carefully, em ploying a cloth or tissue and a suitable solvent. Take care to remove all of the test material and cleaning solvent. Do not use cleaning utensils that may damage the apparatus. Metal cleaning tools must never be used. 9.5 Repeat the determination with a second specimen. If the two viscosity determinations differ by less than 7 %, calculate their mean and report as the high shear viscosity for the material. If they differ by more than 7 %, make a third determination. If no two readings are within 7 % of each other, then the material is not suitable for testing by this test method. 10. Report ,, 10.1 Report the following information: 10.1.1 Reference to this test method, 10.1.2 Type and identification of the product under test, 10.1.3 Type of cone used (0 to 5 P, 0 to 10 P, etc.), 10.1.4 Rate of shear at which the determination was made (in reciprocal seconds), 10.1.5 Temperature at which the determination was made, 10.1.6 Test results in poises, reported to the nearest 1 % of the total range, that is, 0.05 P for 0 to 5 P-cones, 0.1 P for 0 to 10 P-cones, etc., 10.1.7 Any deviation, by agreement or otherwise, from the test procedures described, and 10.1.8 Date of the test. 11. Precision and Bias5 11.1 Precision--On the basis of an interlaboratory test of this test method in which eight operators in four laboratories tested six paints ranging in viscosity from 0.8 to 7.9 P, the 5 Supporting dala are available from ASTM Headquarters. Request RR:D0J1035. 719 DUP05 02 97901 # D 4287 within-laboratory coefficient of variation was found to be 2.2 %, at 40 df. The between-laboratory coefficient of variation was found to be 6.9 % at 34 df. Based on these results, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 11.1.1 Repeatability--Two test results, each the mean of two determinations obtained by the same operator, should be considered suspect if they differ by more than 6.3 % relative. 11.1.2 Reproducibility--Two results, each the mean of two determinations, obtained by operators in different labo ratories should be considered suspect if they differ by mori than 19.9 % relative. 11.2 Bias--Bias has not been determined for this test method. 12. Index Terms 12.1 This test method is indexed under the followinj terms: viscosity--paints/related coatings/materials; viscom eter--ICI cone/plate. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk, of infringement of euoh rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technlcai committee and must be reviewed every five years and If not revised, eitherreapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments witl receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia. PA 19103. i 720 DU PO 502 97902 Designation: D 4302 - SO Standard Specification for Artists' Oil, Resin-Oil, and Alkyd Faints1 This standard is issued under the fixed designation D4302; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapprovaL A superscript epsilon {<> indicates an editorial change since the last revision or reapproval. `Scope . J This specification establishes requirements for compoion, physical properties, performance, and labeling of 'sts' oil, resin-oil, and alkyd paints. 1.2 This specification covers pigments, vehicles, and addi- Requirements are included for pigment identification, tfastness, consistency, and drying time, i.3 Table 1 lists same pigments meeting the lightfastness uirements in this specification. In order to identify other tents that meet these requirements, instructions are mil for test specimen preparation. Test methods for rmining relative lightfastness are referenced. Referenced Documents 2.1 ASTM Standards: '19 Specification for Zinc Oxide Pigments2 185 Test Methods for Coarse Particles in Pigments, ( Pastes, and Paints3 /387 Test Method for Color and Strength of Color Pigments with a Mechanical Muller2 D 476 Specification for Titanium Dioxide Pigments2 p 602 Specification for Barium Sulfate Pigments2 *D 1133 Test Method for Kauri-Butanol Value of Hydro carbon Solvents4 D 1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems5 V> 1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature5 D1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials6 P 2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates5 >2245 Test Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints4 D2369 Test Method for Volatile Content of Coatings5 Jj> 2689 Practices for Testing Alkyd Resins2 D4236 Practice for Labeling Art Materials for Chronic f Health Hazards5 IP 4303 Test Methods for Lightfastness of Pigments Used !| in Artists' Paints5 specification is under the jurisdiction ofASTM Committee D-I on Paint 1'Related Coatings and Materials and is the direct responsibility of Subcomtee D01.57 on Artist Paints and Related Materials. Current edition approved May 25, 1990. Published November 1990. Originally jlished as D 4302 - 83. Last previous edition D 4302 - 88. f. Annual Book ofASTM Standards, Vol 06.02. $ Annual Book ofASTM Standards, Vols 06.01 and 06.02. $ Annual Book ofASTM Standards, Vo! 06.03. Is Annual Book ofASTM Standards, Vol 06.01. 6 Annual Book ofASTM Standards, Vol 14.02. D 4838 Test Method for Determining the Relative Tinting Strength of Chromatic Paints5 E 284 Terminology of Appearance of Materials6 3. Terminology 3.1 Definitions: 3.1.1 Colour Index Name--consists of the category (type of dye or pigment), general hue, and an assigned number given to a colorant in the Colour Index7 as an international identification system. 3.1.1.1 Discussion--For example, the Colour Index Name of one phthalocyanine blue pigment is Pigment Blue 15 (PB 15). 3.1.2 Colour Index Number--a five-digit number given in the Colour Index that describes the chemical constitution of a colorant. 3.1.2.1 Discussion--For example, the Colour Index Number of one phthalocyanine blue pigment is 74160. 3.1.3 Refer to Terminology E284 for appearance terms used in this specification. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 alkali refined oil--triglyceride oil of vegetable origin that has been treated with alkali to reduce the free acidity by formation of water-soluble salts, subsequently removed by washing. 3.2.1.1 Discussion--An appreciable degree of free acidity may cause a greater development of yellowing in a dried film of oil. Most artists' oil paints are grpund in alkali refined oil. 3.2.2 alkyd paint--paint containing a resin produced by combining a polybasic acid, a polyhydric alcohol, and the fatty acid of a drying vegetable oil. For this specification, the resin produced must be soluble in mineral spirits or turpen tine. 3.2.3 drier (siccative)--a substance, usually an organometallic compound, that accelerates the rate of drying of an oil paint or oil medium. 3.2.4 oil paint--paint containing an alkali refined triglyc eride drying oil of vegetable origin. 3.2.5 resin-oil paint--paint containing 90 weight % min imum of vehicle solids, vegetable drying oil, and 10 weight % maximum of vehicle solids replaced by gum or resin. 4. Significance and Use 4.1 This specification establishes quality requirements and provides a basis for common understanding among producers, distributors, and users. 4.2 It is not intended that all paints meeting the require ments be identical nor of uniform excellence in all respects. 7 Colour Index, 3rd ed., 5 Vols and Revisions, The Society of Dyers and Colourists, London, 1971-75. Available from the American Association of Textile Chemists and Colorists, P. O. Box 12215, Research Triangle Park, NC 27709. 721 DUP050297903 # D 4302 TABLE 1 Suitable Pigments List M' --Underlined information and the lightfastness rating in the table shall be included on every label. Key: Lightfastness Category: Lightfastness i Excellent Lightfastness Ughtfastness il Very Good Lightfastness Abbreviations Used in Colour index Names: NR Natural Red P8 Pigment Blue PBk Pigment Black PBr Pigment Brown PG Pigment Green PO Pigment Orange PR Pigment Red PV Pigment Violet PW Pigment White PY Pigment Yellow Pigment Notations: (BS) Blue shade (CC) Concentrated cadmium pigments may contain up to 15 % barium sulfate for color control. Cadmium-barium pigments contain a much higher amount of barium sulfate. (DL) May darken in strong light (LF) Lightfast type (NA} Colour index name or number not (NR) Not rated as lightfastness I or II ... Not tested (RS) Red shade (SM) Sensitive to moisture in direct sunlight (SS) Sensitive to hydrogen sutfide Colour Index Name Lightfastness Category Oil Alkyd Resin-Oil Colour Index Number YELLOWS PY 1, PY1.1 [J il PY 3 II il PY 35 PY 35:1 1 1 PY 37 PY 37:1 fI 1 PY 40 li PY 41 PY 42 1 1 PY 42 PY 43 PY 53 PY 65 PY 73 11 1 1 1 PY74(LF) PY 83 HR 70 PY 97 PY 98 1 1 li PY 108 PY 109 PY 110 PY 112 PY 138 PY 139 PY 150 PY 151 PY 153 PY 154 PY 175 1 1 i 1 1 i 1 1 1 1 1 Arylide Yellow G, with option of adding the name Hansa Yellow Medium, arylide yellow 116B0 Arvllde Yellow 10G, with option of addina the name Hansa Yellow Liqht. arylide yellow 11710 Cadmium Yellow Light, concentrated cadmium zinc sulfide fCCt fSM) 77205 Cadmium-Barium Yellow Light, cadmium zinc sulfide coDrecloitated with barium sulfate (SM) 77205:1 Cadmium Yellow Medium or Deep, concentrated cadmium sulfide fCC) (SM) Cadmium-Barium Yellow Medium or Deep cadmium sulfide copreciDitated with barium sulfate (SM) 77199 77199:1 Aureolin, with option of addina the name Cobalt Yellow, potassium 77357 cobaltinitrite Naples Yellow, lead antimoniate (SS) 77589 I Mars Yellow, with option of addina the name Yellow,^iron Oxide, synthetic 77492 hydrated iron oxide 1 Mars Oranae, synthetic hvdrateti iron oxide f Yellow Ochre, natural hvdrated iron oxide \ hflckd Titanate Yellow, oxides of nickel, antimony and titanium 77492 77492 77788 Arvlide Yellow RN, with option of addina Hansa Yellow RN. arvlide yBilow Arvllde Yellow GX. with option of adding the name Hansa Yellow GX. arylide yellow 11740 11738 Arvlide Yellow 5GX. with option of addina Hansa Yellow 5GX. arvlide yellow 11741 I iarvlide Yellow HR70. diarviide vellow 21108 ' An/lide Yellow FGL, arvlide veliow 11767 Arvlide Yeltow 10GX, with option of addina the name Hansa Yellow 10GX. 11727 arylide yellow 1 Anthrapvrimidine Yellow, anthrapyrimidine 68420 Isolndolinone Yellow G, tetrachloroisoindolinone 1 isoindolinone Yellow R, tetrachloroisoindolinone Fiavanthrone Yellow, flavanthrdne 1 Quinoohthalone Yellow. auinoDhthalone isolndoline Yellow, isdndoline Nickel Azo Yellow, nickel complex azo NA 56280 70600 NA NA NA Benzimidazolone Yellow H4G. benzimidazolone l Nickel Dioxine Yellow, dloxine vellow nickel complex l Benzimidazolone Yellow H3G. benzimidazolone Benzimidazolone Yellow H6G, benzimidazolone 13980 NA 11781 11784 722 DUP050297904 4, Colour Index Name ' PO 5 1*0 20 i. PQ 20:1 f PO 23 'f PO 23:1 PO 36 PO 43 O AS TO i9 * FO 60 i"*p*"oes &FR5 ft PR 7 p PR 9 Su PR 14 FR 8B 9 " * r pn toi fepR 101 \ *R "01 i PR 101 Sp r mi Sf PR 102 & PR 10(3 SKPR 108 X PR 108:1 IK PR 112 PR 113 PPR 113:1 S PR 119 PR 122 PR 123 FR14) fe*PR 168 WPR 170 F3RK-70 PR 170 F5RK f^PR 175 9 n s PV'S W PR 179 ^PR 188 & PR 190 RPB 192 & PR 194 *J PR 207 / ro *4s APV19 ^,PV 14 S^PV 15 fs.PV 15 f/PV 16 f PV 19 fFV23BSfl> L PV 23RSII) fjl PV 31 D 4302 Lightfastness Category Oil Alkyd Resin-Oil TABLE 1 Continued H 1t 11 1 II 11 1 II 1 11 1 1 1 1 1 1 1I II (1 II II II 11 II 11 ORANGES Dinitraniline Orange, dinitranlUne fSM) 1 Cadmium Orange, concentrated cadmium sulfo-selenide (CC) Cadmium-Barium Oranae. cadmium sulfoseienide coprecipitated with barium sulfate Cadmium Vermilion Orange, concentrated cadmium mercury sulfide (CC) Cadmium-Barium Vermilion Oranae, cadmium mercury sulfide coprecipitated with barium sulfate Benzimidazolone Orange HL, benzimidazolone Perlnone Orange, perinone .Quinacridone Bold, ouinacridone Quinacridone Deep Gold, ouinacridone Benzimidazolone Orange HQL. benzimidazolone Benzimidazolone Oranae H5G, monoacetolone REDS Naphthol ITR. nachthol'ITR 1 Naphthol AS-TR, naphthol AS-TR Natural Rose Madder, natural madder Naphthol AS-OL, naphthol AS-OL Naphthol AS-D, naphthol AS-D 1 Thiolndiqoid Violet, thioindigold Indian Red. synthetic red iron oxide (bluish hue) Uqht or English Red Oxide, synthetic red iron oxide (yellowish hue) Mars Red, with option of addina the name Red Iron Oxide, synthetic red iron oxide 1 Mars Violet, with option of addinq the name Violet Iron Oxide, synthetic Iron oxide (violet hue) Venetian Red. synthetic iron oxide (yellowish hue) Uqht Red, calcined yellow ochre Vermilion, mercuric sulfide (DU 1 Cadmium Red Uqht, Medium, or Deep, concentrated cadmium-seleno sulfide (CC) Cadmium-Barium Red Uqht. Medium or Deep, cadmium seieno-sulfide coprecipitated with barium sulfate Naphthol AS-D. naohthoi AS-D Cadmium Vermilion Red Uaht, Medium or Deep, concentrated cadmium mercury sulfide (CC) Cadmium-Barium Vermilion Reef Uqht. Medium or Deep, cadmium mercury sulfide coprecipitated with barium sulfate Naphthol Red. naphthol I Quinacridone Maqenta, y quinacrictone ` Perylene Vermilion, perviene Perylene Red. perviene t Bromlnated Anthranthrone. brominated anlhranthrone Naphthol Red. naphthol carbamide Nachthol Crimson, naphthol carbamide Benzimidazolone Maroon, benzimidazolone 1 1 Perviene Maroon, perylene Naphthol AS. naphthol AS Perylene Red, perylene Quinacridone Red. y quinacridone red Perinone Red Deep, perinone Quinacridone Scarlet, ouinacridone red 1 Quinacridone Red. y ouinacridone red PURPLES 1 Cobalt Violet, cobalt phosphate, cobalt ammonium phosphate 1 Ultramarine Red. complex silicate of sodium and aluminum with sulfur 1 Ultramarine Violet, complex silicate of sodium and aluminum with suifu Manaanese Violet, manaanese ammonium pyrophosphate 1 Quinacridone Violet, auinacridone violet b Dioxazino Purple, carbazole doxazlne Dioxazine Purple, carbazole dioxazine Isovioianthrone Violet, isoviolanthrone Colour Index Number 12075 77202 77202:1 77201 77201:1 11780 71105 NA NA 11782 11775 12490 12420 75330 12460 12380 73312 77491 77491 77491 77015 77491 77492 77766 77202:1 77202:1 12370 77201 77201:1 NA 73915 71145 77137 58300 12475 12475 71513 71130 12467 71140 NA 71100 NA 73900 77360 77007 77007 77742 73900 51319 51319 60010 723 DUP0502 97905 D 4302 Colour Index Name Lightfastness Category Oil Alkyd Resin-Oil TABLE 1 Continued Colour index Number BLUES PB 15 PB 16 PB 22 PB 27 PB 28 PP 29 PB 33 PB 35 PB 36 PB 60 11 l 1 lI 11 11 1 1 1 1 Phthalocyanine Blue, copper phthalocyanine 1 Phthalocyanine Blue, metal free Dhthalocvanine Indanthrone Blue, Indanthrone i Prussian Blue, with the option of adding the name Milori Blue, ferriammonium ferrocyanide 1 Cobalt Blue, oxides of cobalt and aluminum 1 Ultramarine Blue, complex silicate of sodium and aluminum with sulfur 1 Manganese Blue, barium manganate with barium sulfate 1 Cerulean Blue, oxides of cobalt and tin Cerulean Blue. Chromium, oxides of cobalt and chromium s Indanthrone Blue, indanthrone GREENS 74160 74100 69B10 77510 77346 77007 77112 77368 77343 69800 PG7 PG 10 PG 17 PG 18 PG 19 PG 23 PG36 PG 50 !1 1 1 11 1 i1 1 f i Phthalocyanine Green, chlorinated copper phthalocyanine Green Goid, wi.th option of adding the name Nickel Azo Yellow, nickel chelated azo i Chromium Oxide Green, anhydrous chromium sesquioxide Viridian. hydrous chromium sesquioxide i Cobalt Green, oxides of cobalt end zinc l Green Earth or Terra Verte, natural qreen i Phthalocyanine Green, chlorinated and brominated phthalocyanine i Liaht Green Oxide, oxides of nickel, cobalt and titanium BROWNS 74260 12775 77288 77289 77335 77009 74265 77377 PBr 6 PBr 7 PBr 7 PBr 7 PBr 7 1 11 11 11 11 i Mars Brown, with option of adding the name Brown Iron Oxide, synthetic 77499 brown iron oxide or mixtures of synthetic iron oxides i Burnt Sienna, calcined natural iron oxide 77492 Burnt Umber, calcined natural iron oxide containing manganese 77492 Raw Sienna, natural Iron oxide 77492 Raw Umber, natural iron oxide containing manqanese 77492 BLACKS PBk 6 PBk 7 PBk 9 PBk 11 11 1 11 1 Lamp Black, nearly pure amorphous carton Carbon Black, nearly pure amorphous carbon i tvorv Black, amorphous carbon produced by charring animal bones i Mars Black, with option of adding the name Black Iron Oxide, synthetic black iron oxide WHITES 77266 77266 77267 77499 PW 1 PW 4 PW 6 11 1 11 Flake White, basic lead carbonate (SS) Zinc White, zinc oxide Titanium White, titanium dioxide {rutile or anatase) with option of including some barium sulfate or zinc oxide v 77597 77947 ; 77891 A Applies only to Permanent Red Violet MRS, product of American Hoechst Corp.. Coventry, Rl 02816. Pigments described as thiorndigoids have varying degrees of Eightfastness. Variations in manufacture, not covered by this specification, may cause some artists to prefer one brand over another, either of which may be acceptable under this specification. 5. Labeling Requirements 5.1 Pigment(s) Identification: 5.1.1 Every label shall include for each pigment contained in the paint (/) the information underlined in Table 1 (which includes the Common Name, Colour Index Name, and any additional terms necessary to identify the form of the pigment) and (2) the appropriate Lightfastness Category. 5.1.2 The complete pigment identification given in Table 1, which also includes the Colour Index Number and a simple chemical description, shall be given in an appropriate producer publication. Manufacturers are encouraged to put this complete identification on the container label when label size permits. 5.1.3 The Common Name shall be placed on the front of the label and shall be the name of the paint except as described in 5.1.5 and 5.1.6. Other identification may be placed elsewhere on the container. 5.! .4 The Colour Index name may be spelled out in full or. abbreviated depending on the size of the label. Example:!!! Pigment Blue 15, or Pig. Blue 15 or PB 15. 5.1.5 Substituted Pigment--In the case of substitute pigments, the word "Hue" in equal size letters shall follovf to; the title, on the front of the tube, immediately after the name, of the pigment that has been simulated. Directly below the'< title, the Common Name of the significant pigment ustv shall be given in letters no less than the next type size smaller than the title. For example: COBALT BLUE HUE (ULTRAMARINE BLUE). 5.1.6 Proprietary names or optional names may be used. provided the Common Name(s) given in Table 1 appears 0" the front of the label directly under the proprietary t.i optional name in letters no less than the next type si; smaller than the proprietary or optional name. 5.1.7 Mixed Pigments--Artists' paints containing more than one colorant comply with this specification if t 724 DUP050297906 # D 4302 > ilorcd pigments used are on the suitable pigment list (Table 4[' and provided the mixture itself has passed all other test 'H'Cifuirements in this specification. The lightfastness category 11 be that of the least lightfast pigment. This lightfastness Sgory may be changed if these paints are tested for tfastness in accordance with Test Methods D4303 and lilts indicating a different category are submitted to iM Subcommittee D01.57 for evaluation. jf,2 Provide on the label: js.2.1 Artists' Oil Paints--Vegetable origin of the oil and thod of refinement. itoTE 1--The type of oil can be identified in accordance with Test I D 2245. 2.2 Artists' Alkyd Paints--Type of fatty acid used. If vegetable oil is used in combination with an alkyd resin, i this also on the label. State if compatible with artists' its. 2--The type of alkyd can be identified in accordance with : D 2689. 12.3 Artists' Resin-Oil Paints--Vegetable origin and 1 of refinement of the oil and type of resin or gum. If colors in a resin-oil paint line contain more than one, or t, gums br resins, the identification on the individual may uniformly include all of the gums or resins used paint line. Example: "Damar or Mastic Gum." State if "tible with artists'oil paints. 3--The type of oil can be identified in accordance with Test D 2245. ,Lightfastness--The label shall contain the word ness" followed by the appropriate rating, I or II, as for each pigment in Table 1. Lightfastness I pigments, when made into paint ens as described in Section 8 and exposed, tested, and in accordance with Test Methods D 4303, shall have a ^difference (AE*ab) of 4 or less CIELAB units between nens measured before and after exposure. .2 Lightfastness II pigments, when made into paint jjiens as described in Section 8 and exposed, tested, and jin accordance with Test Methods D 4303, shall have a Isfifference (AE*ab) of more than 4.0 but not more than BLAB units between the specimens measured before er exposure. ,3 Pigments were placed in a lightfastness category on : of either known historical performance in art works ratings from four lightfastness tests conducted as in Test Methods D 4303. Results from further tests ese, or other pigments, are solicited by Subcommittee 7- .1 The lightfastness category of a pigment shall be if results from several further tests conducted in ce with Test Methods D4303 and approved by Subcommittee DO 1.57, establish a different lightfastcategory than the one given in Table 1. .3.2 Additional pigments shall be placed in Table 1 jthey have been tested for lightfastness in accordance Test Methods D 4303 and the test results submitted to Subcommittee DO 1.57 for evaluation, provided the : demonstrate that the pigments have the lightfastness "S required for Lightfastness I or Lightfastness II, as "bed above. 5.3.4 For information and to establish nomenclature, pigments in Lightfastness III category are given in Table Xl.l in Appendix XI, but are not to be used in paint conforming to this specification. These pigments have a color difference before and after exposure of more than 8.0 but not more than 16.0 CIELAB units. 5.4 Contents--To be expressed in volumetric measure as required by law. 5.5 Toxicity--All products and labeling must conform to the Federal Hazardous Substances Act and to Practice D 4236. 5.6 Statement of Conformance--"Conforms to ASTM Specification D 4302," or "Conforms to ASTM D 4302," or "Conforms to the quality requirements of ASTM D 4302." This statement may be combined with other conformance statements, such as, "Conforms to the quality and health requirements of ASTM Specification D4302 and Practice D 4236." 5.7 Address--Include on the label (1) the name and address of the manufacturer or importer and (2) the country of manufacture. 6. Quality Assurance for Artists' Oil Paints and Artists' Resin-Oil Paints 6.1, Conditions Not Covered in This Specification that Affect Artists' Oil and Resin-Oil Paints: , 6.1.1 Substrate--Factors such as the texture, gloss, effec tive pH, porosity, chemical composition, and condition of the substrate will affect gloss, gloss uniformity, drying time, adhesion, and the flexibility of the dried film. 6.1.2 Environmental Conditions--Factors such as temper ature, humidity, air flow, and light conditions affect applica tion properties, film formation, drying time, and adhesion. 6.1.3 Storage--With aging and elevated temperatures, there may be a change in consistency and a separation of oil from, the paste paint. 6.2 Vehicles--Only vegetable drying oils shall be used in artists' oil paints. Resin-oil paints shall contain 90 weight % minimum ofvehicle solids, vegetable drying oil {see Note l), and 10 weight % maximum of vehicle solids replaced by gum or resin. 6.3 Pigments--Pigments to be used in oil paints shall be limited to those listed in the column labeled "Oil" and pigments to be used in resin-oil paints shall be limited to those listed in the column labeled "Resin-Oil" in Table 1. Their lightfastness rating shall be the numeral given in the same row. Those pigments listed as "not tested" shall not be used, 6.4 Driers'--Driers may be used in minimal amounts in paints that contain a pigment which has a retarding effect on the drying of oil. This is allowed so these paints can conform to the drying requirements of this specification. 6.5 Inerts--Minimal amounts of inert pigments may be used to produce desirable working qualities and consistency, to prevent separation, to develop chromatic properties, or to ensure the durability of the paint film. 6.6 Preparation of Sample--Empty the contents of a previously unopened container onto a glass slab and mix thoroughly with a spatula to a homogeneous sample. 6.7 Nonvolatile--The nonvolatile content shall not be less than 97 weight % for the oil paints and 90 weight % for the 725 DUPO 50297 907 # D 4302 wmm ? resin-oil paints, as determined by Test Method D 2369. 6.8 Coarse Parlicles--Paints shall be free of oversize particles and shall form a uniform film. The maximum content ofcoarse particles shall be 1 weight % as determined by Test Methods D 185. 6.9 Fineness of Dispersion--On a glass plate, using a spatula, mix the paint with an equal volume of linseed oil until homogeneous. If the paint is very thick, it may be necessary to add a minimum amount of mineral spirits or turpentine to make the paint sufficiently fluid to read the gage accurately. Determine the fineness of dispersion by Test Method D 1210. The maximum allowable grind reading is 1.5 mils (40 pm). 6.10 Consistency--The paste type of paint shall not flow or level when applied with a palette knife. 6.11 Drying--Using a film applicator with a 3-mil (75pm) clearance, make a uniform drawdown on a lacquersealed panel. At a relative humidity of 50 to 75 % and a temperature of 65 to 80F (18 to 27C), the dustfree drying time, as determined by Test Methods D 1640, shall not be more than ten days. 6.12 Tinting strength requirements will be included in this specification as appropriate tinting strength standards for individual pigments are established. Test Method D 387 may be used to determine the tinting strength of pigments or paints when all ingredients are known. Test Method D 4838 can be used to determine the relative tinting strength of chromatic paints containing a single pigment and the same vehicle but where other ingredients are unknown. 7. Quality Assurance for Artists' Alkyd Paints 7.1 Conditions Not Covered in This Specification that Affect Artists ' A llcyd Paints: 7.1.1 Substrate--See 6.1.1. 1A.2 Environmental Conditions--See 6.1.2. 7.1.3 Storage--With aging and elevated temperatures, there may be a change in consistency and possible solvent loss. Some separation of the medium is also possible. 7.2 Vehicles--Only alkyds that are soluble in mineral spirits or turpentine may be used in artists' alkyd paints. Free vegetable drying oils may be included in artists' alkyd paints up to 25 weight % of the vehicle solids. 7.2.1 The amount of yellowing in a vehicle should not exceed the yellowing of a linseed oil paint. To assess exces sive yellowing of the alkyd vehicle or alkyd vehicle/drying vegetable oil blend used in alkyd artists' paints, put the vehicle including its usual drier and all additives in the following formula: Weight % Alkyd vehicle under lesl including driers Mineral spirits Rutile titanium white* {conforming to Type II of Specifica- tion D476) China clay Blanc fixe (conforming toSpecification D 602} Ami-skinning agent 22 !1 30 14 22 1 Non- 4--More or less mineral spirits may be used for ease of brushing. V,7.2.2 Prepare a white oil paint using the same titanium white dispersed in alkali refined linseed oil. Make specimens from the alkyd and oil paints as directed in Test Methods D 4303, and expose them to light filtered through glass using Test Method 1 and either Test Method ,2 or Test Method 3 ns described in the Procedure section of Test Methods D 4303 7.2.3 Following exposure check that the alkyd specimens are the same or less yellow than the oil specimens exposed by the same test method. (Use Practice D 1729 or Test Method D 2244 to determine amount of yellowing.) 7.3 Pigments---Pigments shall be limited to those recom mended for use in alkyd paints in the column labeled "Alkyd" in Table 1. Their lightfastness rating shall be ihe numeral given in the same row. Those pigments listed j, "not tested" shall not be used. 7.4 Driers--Minimal amounts of driers may be used to allow paints to conform to the drying requirements of this specification. 7.5 Inerts--See 6.5. 7.6 Sampling--See 6.6. 7.7 Coarse Particles or Foreign Matter--See 6.8. 7.8 Fineness of Dispersion--On a glass plate, using a spatula, mix the paint with linseed oil in a one-to-one volumetric ratio until homogeneous. If the paint is very thick, it may be necessary to add a minimum amour.: o' turpentine or mineral spirits to make the paint sufficiently fluid to read the gage accurately. Determine the fineness of dispersion in accordance with Test Method DI2I0. The maximum allowable grind reading is 1.5 mils (40 pm). 7.9 Drying--Using a film applicator with a 3-mil t75-uml clearance, make a uniform drawdown on. a lacquer-sealed panel. At a relative humidity from 50 to 75% and'a temperature from 65 to SOT (18 to 27C), the dust-free drying time shall be not more than 2 days or less than 30: min. 8. Lightfastness Determination 8.1 If a pigment is not listed -in Table 1, test specimens of a paint containing the pigment shall be prepared. These t. . specimens shall be tested in accordance with the u.qn ' ments for exposure and evaluation given in Test Methods D 4303. N' 5--A report of the results of these tests may be submitted to* Subcommittee D0t.57 for inclusion of the pigments in Table I. Thereport shall include information on test conditions and instruments used >: and shall be accompanied by test specimens, which will be returnee. 8.2 Materials: 8.2.1 Aluminum Exposure Panelf 3 by 6 in. (75 by T50 mm). 8.2.2 Posterboard, lightweight, approximately 20 mils (0.5 mm) thick, having a glossy finish on one side. 8.2.3 White Soya Alkyd Enamels used to prepare white , ground coats. 8.2.4 White Artists' Paints--Depending on the vehicle in which the pigments are to be tested: 8.2.4.1 Titanium dioxide yellowing-resistant oil paint, x DuPont RyOO Rulile titanium dioxide, manufactured by E. 1. du Ponl de Nemours & Co., 1007 Market St., Wilmington, DE 19898. has been found satisfactory for this purpose. 11 The No. A-36 Aluminum Panel, manufactured by The Q-Pane] Co., 26?fH First St., Clevetand, OH 44145, has been found satisfactory for this purpose. 726 H Jk DUP050297908 # 4302 3.2.4.2 Titanium dioxide yellowing-resistant alkyd paint, .2.4.3 Titanium dioxide yellowing-resistant resin-oil nt 8.2.5 Spray Apparatus, for applying ground coats. 8.2.6 Paint Brush, 2.5 in. {60 mm) wide for applying l coats if spray apparatus is not available. ,2.7 Soft Hair Brush, 1 in. (25 mm) wide for applying land coats to aluminum panels. An oxhair artists' "stroke" sh is suitable. .3 Summary ofMethod: .3.1 Pigments to be tested are dispersed in the appro- vehicle and diluted with a standard mixing white of same type of vehicle until the spectrophotometric meas- ent of the dried'film reads from 35 to 45 % reflectance wavelength of maximum absorption for that pigment. I artists' paints ofknown composition may be tested. 4 Specimen Preparation: 4.1 Ground Coats: 4.1.1 For two ground coats to be used under oil, alkyd, resin-oil paints, prepare the following enamel: Weighl % 'um oil length soya alkyd, 50 % nonvolatile10 tile titanium, chloride? (conforming to Type H of Specif!- Cation D 476) he fixe (conforming to Specification D 602) ers 0.15 % zinc and 0.15 % zirconium as meta) on the alkyd nonvolatile iTicient mineral spirits for milling 20 40 ' 40 ft. 1.2 Mill to a Hegman fineness of 7 as measured by Method D 1210. Thin with mineral spirits to approviscosity for spraying or for flow coating by brush. 6--These soya alkyd enamels are used for the ground coats of their color stability, nonabsorbency, adhesion of the specilsoats under humid conditions, and freedom from blistering that occur with an acrylic ground coat under high humidity. 1.2 Application ofGround Coats: 1.2.1 Degrease aluminum substrates before applying the d coat. j2.2 Under oil, alkyd, and resin-oil paints, apply two of the enamel described in 8.4.1.1 to the aluminum or oard supports, either by spraying or by flow coating a brush. To flow coat the aluminum panels for sun use a I-in. (25-mm) soft-hair brush. Coat the rboard to be used for laboratory exposure on the less ' ent, glossy side. TH 7--Coating the posterboard is most conveniently done on the (Sheet before cutting to size. 2.3 Allow a minimum of five days drying time foltg the first coat and two weeks or more before applying yecimen to be tested. 13 Mixing Whites for Dilution ofColors: .3.1 For oil paints use the following white: ie following alkyd resins have been found satisfactory for this purpose: No. 51-5196; McWhorter. DURAMAC 2409; Reichbold, No. 11-035; Kellog, AROPLAZ 1082 M50. Weight % Alkali refined safflower oil Aluminum distearate Rutile titanium dioxide8 (conforming to Type II of Specifi- cation D476) a Blanc fixe (conforming to Specification D 602) Zinc oxide (conforming to Specification D 79) 22.5 2.0 30.0 39.5 6.0 8.4.3.2 Mill to a Hegman fineness of 7 as measured by Test Method D 1210. 8.4.3.3 Keep the viscosity of the mixing white to 250 P or slightly lower. 8.4.3.4 For diluting alkyd paints use the following white containing two alkyd resins: Weight % Medium oil length soya alkyd,10 62% oil length, 70% nonvolatile, white spirit as-volatile Medium oil length soya alkyd, 62% oil length, 51% nonvolatile, mineral spirits as volatile MineraTspiiits Rutile titanium dioxide6 (conforming to Type II of Specifi- cation D 476) Blanc fixe (conforming to SpecificationD 602) China clay Anti-skinning agent Zinc oxide (conforming toSpecificationD 79) !0 12 11 30 16 14 1 6 84.3.5 Mill to a Hegman fineness of 7 :as measured by Test Method D 1210. 84.3.6 For diluting resin-oil paints, use the following white: Weight Alkali refined safflower oil Aluminum distearate Damar resin dissolved -in 3 % mineral spirits (Note 8) . Rutile titanium dioxide8 (conforming to Type II of Specifi- cation D476) Blanc fixe (conforming to Specification D 602) Zinc Oxide (conforming to Specification D 79) 20.7 2 1.8 30 39.5 6 N ' 8--The kauri-butanol value of the mineral spirits shall be >40 as determined by Test Method D 1133. 84.3.7 Mill to a Hegman fineness of 7 as measured by Test Method D 1210. 8.4.4 Preparation of Test Paints: 84.4.1 The pigment to be tested may be milled in a concentrated paste in a resin-oil vehicle. If a prepared resin-oil artists' paint of known composition is available, it may be used for this test. 84.4.2 Dilute the pigment paste or paint with the white given in 84.3.6 until the spectrophotometrie measurement of the dried film shows 35 to 45 % relative reflectance at the wavelength of maximum absorption for that pigment. The wavelength of maximum absorption is located at the point of lowest reflectance on the spectral curve between 420 and 620 nm. If using a tristimulus filter colorimeter, the lowest of the three filter readings is the region of maximum absorption and the dilution should be adjusted so that a reading of 35 to 45 % reflectance is obtained with this filter. The diffuse white reference standard for all measurements should have an absolute reflectance between 97 and 100 %. 8.44.3 To obtain this reflectance, use the Kubelka-Munk Single Conslant Method described in Appendix X2 or use a trial and error method. 8.4.44 Make instrumental readings with the specular reflectance included to minimize the effect on readings of 727 DUP0502 97909 D 4302 any change in gloss and to minimize the effect of brush strokes. 8.4.4.5 Use an applicator with a 6-mils (150-pm) aperture to make a minimum size drawdown, 1 Vi by 1 Vi in. {40 by 40 mm), or other minimum size appropriate for the viewing area of the instrument used. Return ail recoverable paint to the batch to allow for repeat mixes and measurements. 8.4.4.6 For oil, alkyd, or resin-oii paint, an initial amount of 40 g of white paint is sufficient if specimens .are read wet and recoverable paint is returned to the batch. If the instrument provides a way to read wet paint behind glass, and specimens measured this way fall, within the accepted range when dry, this method can be used. N ( 9--Another suggested method for reading oil paints while wet is to cut from 0.013-mm thick kitchen plastic wrap (such as Saran wrap) the minimum size piece that will protect the instrument and then die-cut a hole in the proper location Vsin. (3.2 mm) smaller than the instrument aperture. Rubbing the plastic several times with a paper towel or tissue imparts sufficient static charge that the protective plastic adheres to the instrument enabling the operator to center the hole on the aperture. The wet oil paint drawdown can then be placed in position, taking earn not to disturb the plastic shield. 8.4.4.7 For the initial weights of white stated in 8.4,3.1, 8.4.3.4 and 8.4.3.6 the weighing must be accurate to 0.05 g. 8.4.5 Application ofPaints to Panels: 8.4.5.1 Prepare four specimen panels on appropriate sub strates for each pigment under test. Two are used in the first lightfastness tests and two are retained in subdued light, one for visual comparisons with the exposed panels and one in case a third test is needed to supplement results from the first two tests, as described in Procedure section Test Methods D 4303. 8.4.5.2 Apply the test paints by brush to the aluminum or posterboard exposure panels described in 8.2, depending on whether exposure is to be under glass to the sun or to laboratory apparatus. 8.4.5.3 Using the No. 12 artists' flat bristle brush, brush the panels lengthwise, then crosswise, and again lengthwise, this time with a light touch to produce a film as smooth as possible. The mixing whites must be fluid enough t01 facilitate leveling, but not have excess vehicle that can affect the test. Do not use thinners. Oil-paint brushouts retain minor striations. Apply two coats to all specimen panels to achieve complete opacity. 8.4.5.4 Allow specimens to dry between coats as described in the Procedure section (Dry-Through or Dry-to-Handle Time) of Test Methods D 1640. After recoating, allow . specimens to dry hard, as described in the Procedure section > (Dry-Hard Time) of Test Methods D 1640, before measuring j them prior to exposure. General guidelines for drying times 3 are one to two months to dry hard for oil and resin-oil paints; ^ three days between coats for alkyd paints; and five days after recoating. 8.4.5.5 When testing alkyd paints, prepare and expose a specimen of the mixing white along with the colored, | specimens diluted with this white. Since the purpose of these,! lightfastness tests is to evaluate any color change in the1? pigments, if the white yellows appreciably during exposure,adjust any color change between unexposed and exposeef colored specimens to eliminate the effect of this yellowing 9. Exposure 9.1 Conduct exposure tests in conformance with I Methods D 4303. Assign lightfastness categories as described ? in Section 8 of Test Methods D 4303. 10. Keywords 10.1 artists' alkyd paints; artists' oil paints; artists' resio-l oil paints; lightfastness; quality requirements; test specimens! APPENDIXES (Nonmandatory Information) XI. LIGHTFASTNESS III XI. 1 The pigments in Table XL! are not sufficiently lightfast to' be used in paints that conform to this specifica tion. These pigments are listed here, solely to establish common terminology. They may be satisfactory when) full strength (without dilution) or with extra protection from exposure to light. Colour Index Name PR 83 PR 83 PR 146 PR 1B1 Lightfastness Category Oil Alkyd III III III III III TABLE X1.1 Lightfastness III Alizarin Crimson, synthetic 1:2 dihvdroxvanthraauinone on alumina base Rose Madder. Alizarin, synthetic 1:2 dihvdroxyanthraqiJinone on alumina base, more dilute than Alizarin Crimson Naphthol Red, naphthoic arylide Thiolndigoid Magenta, thioindiaoid Colour Index Number 58000 56000 12485 73360 728 DUP0502 97910 X2. KUBELKA-MUNK SINGLE CONSTANT METHOD FOR PREPARING PAINT FILMS 40 5% REFLECTANCE X2.1 Prepare a mixture of white and colorant in proporpns estimated to give a paint having a reflectance of 30 to % at the wavelength of maximum absorption. Calculate he concentration of colorant in white in this batch. Cc= wc/w,,+ here: = concentration of colorant, and and Wc = weight of white and. colorant, respectively, used in the batch, raw or brush a film of this paint over contrast paper at a ickness sufficient to give complete visual hiding. X2.1.1 After allowing the film to dry, measure the reflec- ce of this film at the wavelength of maximum; absorption a spectrophotometer or, if using'a colorimeter, the ectance with the filter that gives the lowest reading (Note .1). Calculate the Kubelka-Munk Single Constant Value this reflectance as follows: (K/S)m = [1 - (Rm - 0.04)]2/2(Rm - 0.04) here: fen. = Kubelka-Munk Value, = reflectance measurement of the mixture, made with the specular component included expressed as a decimal value, and = decimal value correction for surface reflectance. jjfbTE X2.1--To speed drying, accelerated methods may be used. It is Itbnmended that water-based acrylic paints be warmed to 50 to 55C 'i h after I h of air drying before measuring the reflectance. Placing (drawdowns of oil paints near fluorescent lamps, for example in the Jpresccut light exposure racks described In Annex A1 of Test Methods 11303, will speed their drying time. X2.1.2 Calculate the Kubelka-Munk absorption coeffiJt for unit concentration as follows: : Kc='(K/S)JCc e Kc = unit absorption coefficient. 2.2 Based on the results of the trial mixture, calculate fconcentration of colorant in white required to give the ' ed 35 to 45 % reflectance at the wavelength of max'3m absorption as follows: Cd = (K/S)w %fKc = 0.4500/K, re Cd = concentration of colorant in white predicted to ,a paint with the desired 35 to 45 % reflectance value. X2.3 Adjust the concentration of the trial `batch so that the concentration of colorant equals Cd. Determine the changes in colorant concentration, AC, as follows: AC = Cd - C, These changes are positive if the trial batch has a reflectance greater than 40 % and negative if the reflectance is less than 40 %. If AC is positive, add more colorant to the trial batch to bring the concentration of colorant to Cd. If AC is negative, add more white to bring the concentration of colorant to Cd. Because it may be necessary to add large amounts of white to correct for concentrations of colorant giving reflectance values far below 40 %, it is usually best to prepare a trial batch expected to give a AC value that is moderately positive or only slightly negative. X2.3.1 For the case where AC is positive, determine the weight of colorant needed to prepare a second batch as follows: &WC =WC- Cd(JKw + Hy/Cd - 1 x (L.F.) where: A Wc - weight of colorant to be added to the trial batch to obtain a corrected batch with a colorant concentra- L.F. = loss factor = weight of paint from trial batch used to prepare the corrected batch/weight of paint pre pared as trial batch, The loss factor, L.F., allows for paint removed to prepare drawdowns, loss by transfer to different containers, etc. This term may be neglected if losses are small compared to the batch size. The other terms are as defined in the previous sections of this appendix. X2.3.2 For the case where AC is negative, the weight of white needed to prepare a corrected batch corresponds to, A W,, =WC- Cd(l#w + y/Cd X (L.F.) where A1FW = weight of white needed to adjust the colorant concentration in the batch to Cd. Other terms are as defined above or in previous sections of this appendix. X2.4 Prepare a paint film from the adjusted batch. After drying, measure the reflectance at the wavelength of max imum absorption. If this value does not fall within 35 to 45 %, repeat X2.3 through X2.4, where Cd now becomes the Cc for the next batch correction. Normally only a single iteration is necessary and a second batch correction will not be needed. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either.reapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your viev/s known to the ASTM Committee on Standards, 1916 Race SL, Philadelphia. PA 19103. 729 DUP050297911 Designation: D 4303 - 91 Standard Test Methods for Lightfastness of Pigments Used in Artists' Paints1 rtf This standard is issued under the fixed designation D 4303; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 Three test methods consisting of exposure to light (natural sunlight or simulated sunlight) filtered through glass are described as follows: 1.1.1 Test Method A--Exposure under glass to the sun, 1.1.2 Test Method B--Exposure to irradiance from artifi cial daylight fluorescent lamps, and 1.1.3 Test Method C--Exposure in xenon-arc lightfast ness apparatus. 1.2 These test methods are used to approximate the color change that can be expected over time in pigments used in artists' paints in normal indoor exposure. N' 1--The color changes that result from accelerated exposure may not duplicate the results of normal indoor exposure in a home or gallery. The relative resistance to change, however, can be established so pigments can be assigned to categories ofrelative lightfastness. 1.3 Lightfastness categories are established to which pig ments are assigned based on the color difference between specimens before and after exposure. 1.4 Color difference units are calculated by the CIE 1976 L*a*b* color difference equation. 1.5 these test methods apply to artists' oil, resin-oil, acrylic emulsion, alkyd, and watercolor paints. 1.6 This standard does not purport to address the safely problems, if any, associated with Us use. It is the responsi bility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 2244 Test Method for Calculation of Color Differences from Instriimentaily Measured Color Coordinates2 D4302 Specification for Artists' Paints: Oil, Acrylic Emul sion, Alkyd, and Resin-Oil2 D5067 Specification for Artists' Watercolor Paints2 D5098 Specification for Artists' Acrylic Emulsion Paints2 E 284 Terminology of Appearance3 E 1347 Test Method for Color and Color Difference Measurement by Tristimulus (Filter) Colorimetry3 1 These test methods arc under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.57 on Artists' Paints and Related Materials. Current edition approved Sepi. 15, 1991. Published November 1991. Origi nally published as D 4303 - 83. Last previous edition D 4303 - 90. - Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 14.02. E 1348 Test Method for Transmittance and Color 1 Spectrophotometry Using Hemispherical Geometry3 E 1349 Test Method for Reflectance Factor and Color 1 Spectrophotometry Using Bidirectional Geometry3 G24 Practice for Conducting Natural Light Exposur Under Glass3 G26 Practice for Operating Light-Exposure Apparati (Xenon-Arc Type) With and Without Water for Exp sure of Nonmetallic Materials4 '' '/ ii 1ft 1 3. Terminology 3.1 Definitions--Appearance terms used in this st are defined in Definitions E 284. ^ V< 4. Summary of Test Methods 4.1 Color measurements are made on specimens that ha' been prepared as directed in Specification D 4302, D 506 or D 5098 depending on the vehicle. The measurements r recorded for comparison with readings made after tl specimens have been exposed. 4.2 Specimens are exposed to light filtered through gla using at least two of the three test methods describee ,j Section 7. 4.3 The pigments are classified by color difference calc lated in accordance with Test Method D 2244. 5. Significance and Use 5.1 The retention of chromatic properties by a pigmei over a long period of yejrs is essential in an artistic paintm Accelerated exposure simulates color changes that mi reasonably be expected. The producer and the user of artistpaints, therefore, can be apprised of suitable pigments. f 6. Apparatus 6.1 Sun Exposure Facilities as described in Practice G 2a using an exposure angle of 45", facing the Equator. 6.2 Xenon-Arc Lightfastness Apparatus as described Practice G 26: 6.2.1 If water-cooled xenon-arc devices are used (Ty AH or BH of Practice G 26), use borosilicate glass inner anil soda lime outer filters to simulate sunlight filtered throuffl window glass. 6.2.2 If air-cooled xenon-arc devices are used (Types C, Dj or E of Practice G 26), use the combination of optical filterff recommmended by the manufacturer to simulate sunlight filtered through window glass. 6.3 Fluorescent Lamp Lightfastness Apparatus, 4 Annual Book ofASTM Standards, Vols 06.01, 08.03, and 14.02. 730 DUPO 50297912 0 4303 terilux F48TI2VLX/HO lamps3 and constructed iri accord. .iincc with instructions given in Annex Al. ' A Spectrophotometer, abridged spectrophotometer or olnrfmeter capable of including specular reflectance in its casurement. I, Procedure jfi 1 Specimens of pigments to be tested in oil, resin-oil, or cyd panels shall be prepared as directed in Specification p -202. Specimens of pigments to be tested in acrylic l 't ulsion paints shall be prepared as directed in Specification 5:098. Specimens of pigments to be tested in watercolors 1 be prepared as directed in Specification D 5067. f.2 Immediately before exposure, measure all test speci8|$bs on a spectrophotometer (see Test Method E 1348 or 1349) or colorimeter (see Test Method E 1347) with the -ular reflection included in the measurement and record. (|se results shall be compared with subsequent readings of ^exposed specimens to calculate color difference, or with "ngs of retained specimens made at the timej of visual jnparison or before beginning corroborative tests to assure there has been no color change in the interval. fJS. 1 Read specimen panels always with the striations in lisame direction and with panels in the samd position. If (design of the instrument allows, three readings .at Tent locations on the panel should be made and the n calculated. If feasible, mark on the'back of the 'men the spot(s) measured, and re-measure these same s following exposure. If it is necessary to store specimens in the dark' for a of time, prior to measurement and exposure, those "contain oil in the vehicle shall be placed in subdued light |ven-days to eliminate any yellowing-of the oil dire to .3 Expose specimen panels to light passing through glass, to natural sunlight or to simulated daylight in labora- {lapparatus. Oil, resin-oil, alkyd, and acrylic emulsion specimens shall be exposed by Test Method A and ' er Test Method B or Test Method C. Watercolors and paints sensitive to moisture shall be exposed by Test ds B and C. -3J1 Test Method A--Exposure Under Glass to Natural kt: .1.1 Mount the specimens on an open type rack and : at 45 angle to the vertical to a total radiation dose of MJ/m2 in accordance with Practice G 24. !i.2 For tests in southern Florida expose panels during "tenths of October through May. If Test Method B--Exposure to Simulated Daylight orescent Lamp Type): J|j2.1 Mount the specimens with the test face 3 in. (75 (tie Verilux lamps manufactured by Verilux, Inc., P.O. Box 1512, Greenwich, 116336. are temporarily not available. Other fluorescent lamps that closely ? daylight may be suitable, and Subcommittee DO 1.57 seeks information ! allow these fluorescent lamps to be recommended. Lamps should have a led color temperature of 6000 500 K and a color rendering index of at ^0 as calculated by Method of Measuring and Specifying Colour-Rendering of Light Sources, International Commission on Illumination (CIE) tion. No, 13.2 (TC-3.2), 1974. Available from the U.S. National Committee .CIE, y Director of Marketing, OEM Division, North American Philips j Corp.. Philips Square CN88Q0, Somerset, NJ 08873. mm) from the plane of the lamps. 7.3.2.2 Unless specified otherwise, expose the specimens to a repeating cycle of 8 h light followed by 4 h dark until the specimen has been exposed to a total radiant energy dose of 1260 MJ/m2. Rotate the specimen panels two positions to the right after each 100 MJ/m2 dose. This test method takes approximately nihe months to complete. 73.2.3 Maintain the ambient room temperature at 24 3C and prevent the test chamber from exceeding room temperature by more than 6C. 73.2.4 Monitor irradiance at the specimen location for total radiation for each rotation period. Measure radiation 1 h after the lamps are turned on and at the end of the period. The mean of these readings in joules per square centimetre (J/cm2) per hour multiplied by the number of hours of radiation gives the J/cm2 for that period. 7,33 Test Method C--Exposure to Simulated Daylight (Xenon-Arc Type): 73.3.1 Mount specimens in unbacked holders avoiding positions that place specimens at the extreme top or bottom of the specimen rack. 7.33.2 Unless specified otherwise, expose specimens con tinuously to a total radiant dose of 1260 MJ/m2 in accord ance with Practice G 26, Test Method C. Maintain the relative humidity in the test chamber at 55 5 % and a black panel temperature of 63 2C. N' 2--When mutually agreed upon, an alternative dark cycle may be employed in accordance with Test Method D of Practice G 26, optical filter combination (c), and test conditions reported. It has been found that Alizarin Crimson, and possibly other pigments, are affected by a light -and dark cycle, owing to the oxidation-reduction effect of titanium dioxide changing valence with the changes from light to dark and vice versa, characteristic of daylight and indoor light. 733.3 When continuously monitoring irradiance with a narrow bandpass radiometer, the dosage at the monitored wavelength may be calculated knowing the total and spectral irradiance from the lamp operating at a specified wattage, usingtheequation: * QcX=3.6(103)fs, ' (1) where: A = wavelength bandpass expressed in nanometres, nm, Qe = radiometric symbol for radiant exposure, J/m2, 3.6 (103) = a constant, s/h, for converting hours to seconds, t = time expressed in hours, h, and Ec = radiometric symbol for irradiance, W/m2. N' 3--1 W = 1 J/s. N' 4--An example is given in Appendix XI. 7.4 Measure test specimens immediately after exposure with specular reflection included in the measurement and record. 7.5 Calculate the color difference between the specimen before exposure and after exposure in accordance with the CIE 1976 L*a*b* color difference equation in Test Method D 2244. State the color change in total color difference units (4E*ab>. 7.6 Visually check the exposed specimen against the unexposed specimen of the same paint kept in subdued light, in order to verify that the color difference stated in AE*ab units agrees with visual assessment. Make this check also 6 731 : DUP050297913 D 4303 following any subsequent exposures. 7.7 Since all test methods can produce aberrant results in pigments that are sensitive to some aspect ofa particular type of exposure, assign pigments to lightfastness categories based on results from a minimum of two of the methods described in 7.3.1 through 7.3.3. Four exposures arc preferred but there may be fewer in many cases using the following procedure: 7.7.1 Unless specified otherwise, expose one specimen inland outdoors under glass to sunlight in southern Florida below 27" latitude following Test Method A and expose the second specimen indoors to simulated daylight following either Test Method B or Test Method C. Place pigment in the appropriate category if both tests indicate the same category and neither result is within 0.5 AE*ab of the borderline between categories. 7.7.2 If the results, from the first two tests place the pigment in different lightfastness categories, or ifeither of the test results fall within 0.5 AE*ab of the dividing line between two categories, either assign the pigment to the poorer of the two categories involved or for a more accurate rating, proceed with the third exposure. The third exposure may use either the method not used in the two previous exposures, or may repeat the exposure which gave the poorer result, providing the two- test results are within 4 AE*ab of one another. To guard against accepting an aberrant test result, if there is more than 4 AE*ab difference between the first two test results, use the method not employed in the first two tests for the third exposure. 7.7.3 Calculate the mean of the color differences from the three exposures to determine the appropriate lightfastness category unless one of them differs from the nearest test result by more than 4 AE*ab, or the mean is within 0.5 AE*ab of the dividing line between categories. In these cases make a fourth exposure. 7.7.4 For the fourth exposure use the method not previ ously employed, or if all three methods have been used, for the fourth exposure repeat the method with poorest result, unless the results from that method differs from the nearest other test result by more than 4 AE*ab. In this case, discard this one test result. Calculate the mean of the test results from the four exposures, or three exposures if one has been discarded, to determine the' lightfastness category. 8. Interpretation of Results 8.1 Lightfastness I--Assign pigments that exhibit a mean color change of 4 or less AE*ab to Lightfastness Category I. 8.2 Lightfastness II--Assign pigments that exhibit a mean color change of more than 4.0 but not more than 8.0 AE*ab to Lightfastness Category 0. 8.3 Lightfastness III--Assign pigments that exhibit a mean color change of more than 8.0 but not more than 16 q to Lightfastness Category III. 8.4 Since some exposed specimens have lost all color at a color difference of 20 units, additional categories are not appropriate for artists' paints. 9. Report 9. Materials Tested--Report the pigment tested, the name of the manufacturer, and the vehicle used in the test 9.2 Exposure--Report the methods of exposure and their' duration. 3 9.2.1 For Test Method A, in addition to the requirements of Practice G 24, report the total radiation dose in MJ/np;1 9.2.2 For Test Method B, identify the apparatus user1 including types and numbers of lamps, specimen to lamp " Al.l 1uoresc Al.l an | ides tt irger si AL2 distance, panel rotation sequence, light-dark cycle, method of monitoring radiation, exposure dosage in MJ/m2, and teh pparat fumin chamber and room temperature. ad tl: 9.2.3 When using Test Method C, report as directed m iprdbc Practice G 26. Tpparaj 9.3 Test Results--Report AE*ab for each pigment and tha , lightfastness category to which each is assigned. eversd '.ithai 10. Precision 10.1 Variation in test results can result from differences in h<| -ini pigment manufacture from time to time within a comp, different varieties of a pigment from company to compahj" specimen preparation, different instruments and instrJi mental readings, variations in the surface of the spedmeff; and the conditions ofexposure. Allowance for these variables is made by requiring more than one test and by establishing .lightfastness categories that include a range of color differ' ences. 10.2 To establish the relationship between test methods,^ sets of 172 paint specimens, 90 in oil and 82 in aciyae emulsion vehicle, were made at the same time by one; u' and exposed in four sets of lightfastness tests: southern .IsMBS Florida sun filtered through glass, Kansas sun fib', through glass, fluorescent apparatus, and Xenon-arc ratus. rr 10.2.1 All four tests placed 73 % of the pigments i same category. When 12 aberrant test results were dropp. 1 from consideration and the third and fourth expc conducted as required in cases where test results are nei border line between lightfastness categories (see 8.2 combinations of the test results placed 99 % of the pignu- in the same category. 11. Keywords 11.1 fluorescent exposure test; lightfastness; pigment! exposure test. Type C, D, and E; xenon-arc. exposure t 732 DUP050297914 <P D 4303 ANNEX (Mandatory Information for Test Method R) AI. FLUORESCENT DAYLIGHT LAMP LIGHTFASTNESS APPARATUS Ai.l The apparatus for exposing paint specimens to Ifluorescent irradiation is shown in' a large, size version id Fig. jjXi.l and in a smaller version in Fig. Al .2. Figure A1.3 pro-1 |vides the dimensions and arrangement for constructing the ||arger size apparatus out of materials that are easily available. A 1.2 Cabinet Construction--Make framework for the Apparatus out of 1 Vi by 1 lh by 'A-in. (40 by 40 by 3.2-jnm) faluminum angle available in hardware stores. The supports nd the remainder of the enclosure are Vi-in. tempered gjhardboard. The exposure panel supports, which are, also the japparatus sides, are made removable by being fastened by the reversed bolts with wing nuts. Coat them on the interior side path a non-yellowing white paint. Four reflectors, which each n hold four fluorescent lamps, are fastened together by the {1 'ri-in. angles, back to back, to form a square in the center of i e abinet facing the specimens, which are attached to the a.dhoard panels support as shown in Fig. A 1.3. Construct N' --Notice hole for mounting Eppiey pyranometer which is attached at right. (0) Four-Bank Verilux Fluorescent Exposure Apparatus with One Panel Open FIG. A1.1 Apparatus for Exposing Paint Specimens to Fluorescent Irradiation Continued the framework so that the lamps are 3 in. (75 mm) from the test specimens. Cut holes in each side adjacent to the center and centered on a panel location to accommodate an Eppiey pyranometer. With one panel space missing on each panel sun bank, the cabinet accommodates 108 test panels. A 1.3-Irradiation--The reflector fixtures hold sixteen 48 in. (!.2 m) long high powered Verilux6 lamps with a correlated color temperature of 6000 K and a spectral irradiance simulating sunlight. A1.3.1 Irradiance can be monitored by a spectral radiom eter or a filter radiometer which has been calibrated to provide information on the total spectral radiant exposure. N' --Pyranometer, recorder, and demand readout meter In place. (a) Pour-Bank Fluorescent Exposure Apparatus that Handles One hundred and eight 3 fay 6-in. Panels FiG. A 1.1 Apparatus for Exposing Paint Specimens to Fluorescent Irradiation Verilux F48T12VLX/HO lamps have recessed double contact sockets and use a four gang fixture, Series 152 industrial Fixture for Four High Output Lamps. Both are manufactured by Verilux, Inc., P.O, Box 1512, Greenwich, CT 06836. The lamps are temporarily not available. 733 DUP050297915 0 4303 V j* & K- NOTE- -Pyranometer, recorder, and demand readout meter in place. FIG. A1.2 Single-Bank Device ot Four Verilux Daylight Fluorescent Lamps that Handles Twenty-seven 3 by 6-In. Panels A 1-3.2 Install a timer, shown as K. in Fig. A1.3, to cycle exposure for 8 h of light followed by 4 h of dark. Al.3.3 Install an electric time meter in the circuit, shown as N in Fig. A1.3 to record the total amount of time the lamps are turned on. A 1.4 Temperature and Humidity Control--Install a cen trifugal blower unit at the base of the cabinet, shown as I in Fig. A1.3. The air from the blower passes immediately through an air filter O and, after passing through the specimen exposure area, is vented out through the top of the cabinet. The blower furnishes the filtered air draft that keeps the temperature in the cabi net to within 6'C of the ambient temperature of the room. The small 6C temperature rise is sufficient to limit the humidity in the cabinet to about 60 % relative humidity even when the general humidity is vefy high. Install a thermometer in the top of the cabinet near the vent and away from any direct illumination from the lights A1.5 If preferred, a smaller open apparatus holding a single bank of four Verilux daylight fluorescent lamps may be constructed as shown in Fig. A 1.2. A small fan blowing through the unit from one end furnishes the air draft, feu. otherwise the apparatus must have the same distance be tween lamps and specimens and the same monitoring equipment described in A4.2 and A1.3. 734 DUP050297916 # D 4303 Fluorescent Daylight Lamp Apparatus Showing One of Four Sides fe------------- M k------------- 22-"----------------si End view of panel support and side enclosure wing: 1 in. 25 mm. 13-in. distance from lamp to exposure specimen jFour-gang fixture for fluorescent lamps ^Exposure specimens V/2 by 1V? by Ve-in. aluminum angle frame $1 by Vs-in. metal trim strip ?>Win. carriage bolt. %-in. long, spaced 6 in. apart, with wing nut f-Melal comer moulding reversed ^Aluminum angle frame throughout I Centrifugal blower J Fluorescent lamps in 4-gang fixture K Timer to control cycles L Two 2-way switches for Off-On and Interval-On M individual switches for each bank N Time meter O Air Filter, inside P Vent ''N' --Frame is 1 vfe by 1 Va by Ve-in. aluminum angle. Enclosure and removeable panel support sides are tempered hardboard. FIG. A1.3 Dimensions for Constructing Apparatus 735 DUP05029791 7 9 D 4303 [t APPENDIX (Nonmandatory Information) XI. EXAMPLE OF DOSAGE CALCULATION X1.1 The calculation is as follows: Given: Total dose, QT = 1260 MJ/m2 Assume: Total irradiance, , = 1000 W/m2 Spectral irradiance, Ex -- 0.5 W/m2 (XI.1) where A = wavelength of measured spectral irradiance. 0T = 3,6 (103) t Et 1260 (106) = 3.6 (103) t (1000) so t = 1260 (106}/3.6 (10s) = 350 h Thus, if the total irradiance from an energy source remains constant at 1 kW/m2, 350 h are required to provide a total dose of 1260 MJ/rn2. XI.2 If the spectral irradiance at wavelength, A, remains constant, then the spectral irradiation, Qx, or the control dosage, is calculated by the equation, as follows: 2 = 3.6 (103) t E,, 2 = 3.6 (103) 350 (0.5), 2a = 630 (103) J/m2, or 2a = 630 kJ/m2. X1.3 The time required to obtain this dosage may be varied by varying the spectral irradiance. For Ex -- 0.25, the exposure time will double to 700 h. XI.4 If the fluorescent lamp system requires nine months to accumulate 1260 MJ/m2 when the lamps operate two thirds of the time, about 4380 h, then the mean irradiance from the lamps would be: Ey = 1260 (106)/3.6 (103) 4.38 (I03) = 75.1 W/m2 (X1.3) The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if nof revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed fo ASTM Headquarters. Your comments will receive careful consideration at a meeting o`f the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. it m i*i f 736 DUP050297918 Designation: D 4359 - 90 Standard Test Method for Determining Whether a Materia! Is a Liquid or a Solid1 This standard is issued under the fixed designation D 4359; the number immediately following, the designation indicates ihe year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {) indicates an editorial change since the last revision, or reapproval. siope 1.1 This test method covers the determyiation of whether viscous material is a liquid or a solid for regulatory 1 oses. .2 The values stated in inch-pound units are to be Jed as the standard. 1.3 This standard does not purport to address the safety ems associated with its use. It is the responsibility ofthe of this standard to establish appropriate safety and h practices and determine the applicability ofregulatory ations prior to use. ferenced Documents 1 ASTM Standards: 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 :300 Practice for Sampling Industrial Chemicals3 mmary of Test Method The material under test is held at IOOF (38C) in a 'y closed can. The lid is removed and the can inverted, flow of the material from the can is observed to ine whether it is a solid or a liquid. ificance and Use Compliance with regulations often requires the deteration of whether a material is a liquid or a solid. A 'ar test is used by the U. S. Department of Transportafor this purpose. Apparatus si Can, quart (1 L), friction top with lid, diameter ximately 4'A in. (108 mm), height 4% in. (120 mm). 2 Oven, maintained at a temperature of 100F (38C). 3 Tripod or Ring Stand. 4 Watchglass, fared. 5 Stopwatch. 6 Ruler. This test method is under the jurisdiction of ASTM Committee D-l on Paint r< slated Coatings and Materials and is the direct responsibility of Subcom- D01.22 on Health and Safety. nl edilion approved May 25, 1990. Published July 1990. Originally led as D 4359 - 84. Last previous edition D 4359 - 84. Annual Book ofASTM Standards. Vol 06.01. nnual Book ofASTM Standards, Vols 06.03 and 15.05. 6. Sampling 6.1 Using standard sampling techniques, secure a repre sentative sample from the lot or batch being tested, in accordance with Practices D 3925 or E 300. 7. Test Specimen 7.1 If the sample is supplied in a friction top quart can that is at least 85 % full, use the can and material as supplied. 7.2 If not, place the material to be tested into the quart can, filling it to at least 85 % and allowing enough ullage for expansion of the material without displacement of the cover. Tightly close the can so that no vapor escapes. N' --The can is considered 85 % filled when the material level is no more than !h in. (20 mm) below the lip of the can. 8. Procedure 8.1 Place the can with the material in an oven maintained at 100 5F (38 3"C). Allow the contents of the can to come to temperature equilibrium (18 to 24 h). 8.2 Place the tripod or ring stand on a level surface. 8.3 After the material has come to temperature equilib rium take the can from the oven and immediately remove the lid. With the ruler, measure the distance from the surface of the material to the top of the lip of the can and record. 8.4 Invert the can onto the tripod or ring stand in a vertical position over the tared watchglass. If a skin has formed on the surface of the material, break the skin prior to inverting the can. Determine the flow of the specimen out of the can at the end of 3 min, by measuring the vertical distance the material has flowed from the lip ofthe can to the tip of the specimen. 8.5 Add the distance from the surface of the material to the top of the lip ofthe can (8.3) to the distance the material has flowed below the lip of the can (8.4). 8.6 If there is an appreciable flow from the can before the 3 min are up, that is, more than 2 in. (50 mm), immediately stop the test and place the can in an upright position. 8.7 Collect any free-flowing material onto the tared watchglass and weigh. 9. Interpretation of Results 9.1 A material that flows a total of 2 in. (50 mm) or less within 3 min is considered a solid. Otherwise, it is considered a liquid. 9.2 If 1 g or more of liquid is collected on the watchglass, the viscous specimen is considered a liquid regardless of its flow characteristics. 737 DUP05029791 9 4359 10. Precision and Bias 10.1 Precision--II is not practical to specify the precision of this procedure as the results ofthe test are reported only as the state of the material under test. 10.2 Bias--Since there is no accepted reference material suitable for determining the bias, no statement is made. 11. Keywords 11.1 regulations; sample definition;'viscous material char acterization The American Society tor Testing and Materials takes no position respecting the validity ot any patent rights asserted in connection with any item mentioned in this standard. Usees of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, ff you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 738 DU P050297920 Designation: D 4361 - 89 Standard Test Method for Apparent Tack f Printing inks and Vehicles by the Inkometer1 This standard is issued under the fixed designation D 4361; the number immediately following the designation indicates the year of original adoption or, in the case of revision,, the year oflast revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. ^cope I This test method covers the procedure for determining ' apparent tack of printing inks using a mechanical or tronic model of the Inkometer. .2 This test method is applicable to paste-type printing $ and vehicles that are essentially nonvolatile under dinary room conditions. I, 3 This standard mqy invoke hazardous materials, oper3^ and equipment. This standard does not purport to m0ss all ofthe safety problems associated with its use. It is Jtresponsibility of the user of this standard to establish opriate safety and health practices and determine the licability ofregulatory limitations prior to use. .rmiuology :i. Descriptions of Terms Specific to This Standard; II.1 tack--a function of the force required to split a thin dfilm of a printing ink or vehicle between two rapidly abating surfaces; it is a rheological parameter indicative of 'mal cohesion of the fluid. .1.1.1 Discussion--Tack of a printing ink or vehicle is ia fixed number but varies with operating conditions, arily separation velocity, splitting area, and film thickk Tack also varies with changes in the rheological jfprties of the ink or vehicle due to time, temperature, and |ractions with the separating surfaces. In practice, one or % of these surfaces usyally consist of rubber-like rollers sJ,tiiffer :in composition and geometry and whose propertenc to ehatige with age, nature of previously run fluids, '*;df wash-up' solvent; and mechanical flaws. On labora- mstruments, tack readings are also sensitive to the ibratton and zero accuracy of the tackmeter employed. W.2 apparent tack--a tack reading obtained at a specific of conditions. ,i.3 flying--the tendency of a printing ink or vehicle to ejected, as large globules from a roller distribution system. 2.1.3.1 Discussion--Flying is generally most severe ng rapid roller acceleration such as occurs when Ehing immediately from zero or a slow speed to a high "fating* speed. J1.4 misting--the tendency of a printing ink or vehicle to ejected as a fine aerosol from a roller distribution system. 2.1.4.1 Discussion--Misting is generally most severe at ITtais test method is under the jurisdiction of ASTM Committee D-l on Paint [Related Coatings and Materials and is the direct responsibility of Subcom- D01.56 on Printing Inks. Subcommittee D01.37 on Ink Vehicles assisted in development of the vehicle portion of this test method. Current edition approved Oct. 27, 1989. Published December 1989. Originally fashed as D 4361 - 84. Last previous edition D 4361 -84. high operating speeds and with fluids that produce long filaments. 3. Summary of Test Method 3.1 A thin film of the test printing ink or vehicle is applied to the three-roller distribution system of the Inkometer, which operates at speeds comparable to those on production printing presses. Measurement of the frictional torque in duced by drag forces in the splitting film provides an arbitrary value for apparent tack. On mechanical model?, the torque is determined with a manually balanced lever arm, a direct-reading attachment, or a recorder; on electronic models, with a digital readout, recorder, or printer. Readings are in units of gram-meters (g-m). 3.2 The procedure in this test method is designed to give a single value for apparent tack at a specific set of Inkometer conditions. Typical conditions are as follows: a cooling water temperature of 90"F (32.2C); a volume of 1.32 mL (film thickness 12.3 pm) of the test printing ink or vehicle applied to the rollers; an operating speed of 400 r/min for vehicles, 800 r/min for sheet-fed offset inks, and 1200 r/min for web-fed inks;- and a reading after 1 min of operation. Alternative conditions may be used by agreement between the supplier and the customer. 3.3 Instructions are also given for calibration of the Inkometer and for minimizing effects of interactions among the rollers, test fluids, and wash-up solvents. 4. Significance and Use 4.1- Tack of printing inks controls their high-speed transfer properties, as manifested by throughput in roll milling, picking of paper during printing, and wet trapping in multicolor printing. Although an apparent tack measure ment does not completely predict the transfer performance of an ink or a vehicle, it provides a meaningful parameter for quality control, development, and research. 4.2 A given Inkometer will produce repeatable results on a day-to-day basis only if proper attention is paid to calibration and maintenance procedures and to control of experimental variables referred to in 2.1.1.1. 4.3 Two or more Inkometers may not produce identical apparent tack readings, but if each gives repeatable results, they may be mathematically correlated. N ' I --Besides the Inkometer, a number of three-roller tackmeters are available which differ in design features such as roller weight, geometry, and composition. It cannot be presumed that test results from these other types of tackmeters will either agree or correlate with those from the Inkometer. 739 DUP050297921 D 4361 5. Interferences 5.1 Inkometer Squeal--A high pitched whine or squeal may be noted when running high tack fluids or at high rotating speeds, or both. Inkometer squeal may result in instability of the balance beam or direct reading attachment of the mechanical Inkometer or fluctuation of the digital readout of the electronic Inkometer, making definite read ings difficult. 6. Apparatus 6.1 Inkometer2--one of five models differing in available speeds and type of readout as follows: 6.1.1 Mechanical Models B-453, C-453, or MBC, oper ating at fixed speeds of 400, 800 and 1200 r/min on the B-45; 400, 1200, and 2000 r/min on the C-45; and 400, 800, 1200 and 2000 r/min on the MBC. A direct reading attachment2 or a recorder2 is recommended to supplement the manually operated balance beam. 6.1.2 Electronic Models 10I-A3 or 101-8, operating at variable speeds ranging from 100 to 2000 r/min on the 101-A and from 100 to 3000 r/min on the 101-B. A recorder2 or printer2, or both, are recommended to supple ment the digital readout. N!"' 2--To convert to units of linear.speed, multiply Inkometer revolutions per minute by 0.785 to obtain feet per minute or by 0.004 to obtain metres per second. 6.2 Inkometer Rollers,2 of suitable composition, prefer ably one set for each major system to be evaluated (see 10.3.1.) A set consists ofa top (measuring) roller 3'/s in..(79 mm) in diameter and 61/s in. (155 mm) in length, and a vibrator 2.0 in. (51 mrh) in diameter and 1'U in. (184 mm) in length. Together with the fixed brass roller, the total surface area of the distribution system is 166 in.2 (0.107 m2).- The measuring roller weighs 9.2 lb (4.2 kg) on mechanical models and 9.6 lb (4.4 kg) on electronic models. 6.3 Ink Pipet, consisting of a metal cylinder and a metal or' TFE-fluorocarbon plunger. Suitable pipets include the fixed-volume Inkometer pipe,2 1.32-mL capacity; and vari able volume micropipets,'' 2-mL capacity, accurate to 0.01 mL. 6.4 Stopwatch or Timer, accurate to 1 s. 6.5 Ink Knife, small, free from nicks and rough edges. 6.6 Manufacturer's Calibration Apparatus,2 for the spe cific model Inkometer. 7. Reagents and Materials 7.1 Wash-Up Solvent, compatible with the test system, fast evaporating, and having minimal effect on the rollers; it should be acceptable environmentally. Hydrocarbon sol vents with an initial boiling range of 250 to 350F (120 to 177"C), a final boiling range of 300 to 400'F (150 to 205C), a Kauri-Butanol value of 30 to 40 and less than I % benzene content are appropriate for many sheet-fed and heat-set 2 Available from Thwing-Albert Instrumcni Company, 10960 Dutton Rd.. Philadelphia, PA 19154. J No longer manufactured. `Available front I.G.T Reprotesl B.V., J004 Berlin, Cherry Hill, NJ 08034, Pantone, Inc.. 55 Knickerbocker Rd., Moonachic, NJ 07074, or Eastern Scientific, 1459 Lower Ferry Rd., Trenton. NJ 08618. systems. Specific solvents may be required for unique systems. 7.2 Rags or Wipers, clean, soft, absorbent, lint-free. 7.3 Manufacturer's Current Manual?-, for the specific model Inkometer. 8. Hazards 8.1 Never let an ink or a vehicle dry completely on the rollers of the Inkometer. 8.2 Caution--Never turn the ZERO button except during the calibration process (see 12.2.1). 8.3 Take care not to damage the rollers during the cleaning process or by leaving them in contact when the instrument is not in use. 8.4 Do not disengage the balance beam of the mecham,a, Inkometer except when taking a reading. 9. Sampling and Test Specimen 9.1 Carefully select a sample that is free of skin and other contamination and representative of the, lot being evaluated A minimum of 3 to 4 mL is sufficient for two specimens Transfer to a clean container, protect with skin paper, ckr-c and seal. 9.2 When ready to make a run (see 12.3), fill the ink pipet as follows: Transfer 1.5 to 2 mL of sample to a clean glass plate; close and reseal the container. Gently work up with at ink knife but do not aerate. Fill the ink pipet with 1.32 mL of the worked sample (or with a smaller volume (0.5 to 1.0 mL) if a thinner film thickness is desired). Use the ink knife to force the specimen into the cylinder while slowly pulm G back the ram. Wipe excess material off the top of the pi vi N#$' 3--A specimen volume of J.32 mL. divided by:the roller surface area of 0.107 m2, gives an initial film thickness of 12.3 pm when distributed uniformly on the roller system of the Inkometer. Howi the occurrence of appreciable flying or misting will result in \oiv t specimen from the rollers. Hence, operating film thickness is unknown. 10. Preparation and Conditioning of the Inkometer 10.1 Locate the Inkometer on a sturdy bench in % draft-free temperature-controlled environment, preferably 73.5 3.5F (23 2C). Humidity, control is necessary for test samples that arc moisture-sensitive or prone to mistingy 10.2 Set the Inkometer water bath at 90,0 + 0.2"F (32.2 x , O.rC). All tests are to be run at this temperature. (See aK Annex A1.3.) 10.3 Prior to use, ascertain the nature of the test sample for the following reasons: 10.3.1 Roller conditioning--Use only an Inkometer having rollers well broken in for the type of test system. The break-in procedure is given in Annex A 1.2. A separate set of broken-in rollers is mandatory for radiation curing systems. The necessity for separate sets of broken-in rollers, or for extensive reconditioning when switching among different types of conventional test systems shall be determined in each laboratory. 10.3.2 Operating speed--Vehicles are most commonly run at 400 r/min, alternatively at 800 r/min; sheet-fed inks at 800 r/min, alternatively at 400 or 1200 r/min; and web-fed inks at 1200 r/min, alternatively at 800 or 2000 r/min. (The conversion to linear speed is given in Note 2.) 740 ,ioy korr >10.4 ilinj :the dHO q 1' DUP050297922 4 Prior to the first use of the day, equilibrate the eter as follows: 4.1 Warm up the instrument by activating the water g system. Engage the two composition rollers and run . lowest available speed for about 30 min. 1.2 Make a conditioning run with a specimen repre"ve of the system to be evaluated. Apply 1 to 1.5 mL of k or vehicle, and run for 5 to 10 min at the specified eed (see 10.3.2). Clean up as directed in Section 13. Iibration of the Inkometer 1 Calibrate the Inkometer before initial use and pen ally as needed. First, conduct the necessary steps in 10.3 10.4. .2 Using the manufacturer's calibration apparatus, w the directions in the instrument manual. ,2.1 Mechanical Models--Zero and calibrate the bal- beam (and direct reading attachment or recorder, if are to be used) at the test speed specified in 10.3.2. jH.2.2 Electronic Metals--Zero and calibrate the digital out (and recorder, if it is to be used) at 1000 r/min. n calibration is completed, check the dry reading at the |hed test speed (see 10.3.2). O%' 4--The Inkometer can be calibrated at only one speed. 1f.3 After each calibration or at regular periods, .make a fun with a standard ink or vehicle. (See Annex A 1.5.) /Procedure for Tack Evaluation , 0.1 If necessary, make preparations as in 10.3 and 10.4, calibrate the Inkometer as in Section 11. If using an tronic model, make sure the motor is preset to the test d specified in 10.3.2 and the drive is in the LOW mode. 2 Engage the rollers and run at the specified test speed, e .dry reading differs from zero by more than 0.5 g-m, ban the rollers in accordance with 13.1 or recalibrate in Urdance with Section 11. 2.2.1 The dry reading on a properly calibrated instrunt is directly related to the condition of the top (mea' g) roller; therefore, large deviations from zero are ect. Usual causes are inadequate cleaning, residual pie or wash-up solvent, or mechanical damage. Do not 'the ZERO button, as doing so will shift the scale. Do not fnpt to compensate by subtracting the dry reading from test reading. Always reclean or recalibrate. Should large rations from zero persist, contact the manufacturer about possibility of serious mechanical damage. 2.3Turn the Inkometer off, disengage the rollers, and fill pipet as in 9.2. Transfer its contents to the vibrator in a s of thin ribbons around the middle 5 in. (125 mm) of roller. Wipe any specimen remaining in the pipet onto a place on the same roller. Reengage the rollers. 2.4 Distribute the specimen on the rollers and start the as follows: 12.4.1 Mechanical Models C-46 and B-45: 12.4.1.1 Manually turn the motor coupling about ten Volutions, or until the specimen appears evenly distributed ong the three rollers. 12.4.1.2 Set the gears at 400 r/min, start the motor and stopwatch simultaneously, and let the ink distribute for s. Stop the motor but not the stopwatch. 12.4.1.3 Quickly switch the gears to the test speed (spec ified in 10.3.2) and immediately restart the motor, noting the time on the stopwatch. 12.4.2 Mechanical Model MBC: 12.4.2.1 Place the fingertips against the sides of the brass roller and manually turn about ten revolutions, or until the specimen appears evenly distributed among the three rollers. Do not touch the surface of the rollers. 12.4.2.2 Place the speed control switch at the 150 r/min position. Simultaneously depress the power switch on the Inkometer and start the stopwatch. Let the ink distribute for 15 s. 12.4.2.3 Quickly reposition the speed control switch to the test speed, noting the time on the stopwatch. 12.4.3 Electronic Models: 12.4.3.1 Place the fingertips'against the sides of the brass roller and manually turn about ten revolutions, or until the specimen appears evenly distributed among the three rollers. Do not touch the surface of the rollers. 12.4.3.2 Depress the DRIVE button and simultaneously. activate the stopwatch. Let the ink distribute for 15 s at the automatic LOW speed of 150 r/min. 12.4.3.3 Quickly switch to the test speed (preset in 12.1) by depressing the HIGH/LOW button again, noting the time on the stopwatch. 12.5 After 60 s of running at the test speed, record the apparent tack of the test specimen from the balance beam (see Annex A1.4); direct-reading attachment, or the recorder of a mechanical Inkometer or thb digital readout, recorder, or printer of an electronic Inkometer. 12.6 Optional--Rather than restrict the test to a single apparent tack determination, valuable information riiay, in some cases, be gained by continuing the run, taking readings at uniform time intervals (facilitated by the use of a recorder) until the apparent tack begins to decrease. Alternatively, the Inkometer speed may be varied stepwise and a tack reading taken after a specified time at each speed. 12.7 After the run, stop the Inkometer and clean up, as directed in Section 13. : 12.8. Make a replicate test with another specimen of the same sample by repeating 12.2 through 12.6. The two tests should agree within the repeatability given in Table 1. 13. Wash-up Procedure 13.1 With the Inkometer running at the lowest speed, apply a small amount of wash-up solvent to the rollers. Remove most of the specimen from the system by placing pads of the clean, soft, absorbent lint-free rags or wipers firmly against the bottom of the brass roller. Repeat this procedure with additional solvent and pads until the rollers are free from ink or vehicle. If any material remains on the edges of the composition rollers, remove very gently with a solvent-moistened rag. N&'' 5: Caution--Remove material directly from the measuring or vibrator rollers with extreme care. Undue pressure will cause uneven wear of the rollers and may place significant strain on the torsion bar of the electronic Inkometer. Use extreme care to ensure that the cleaning pad does not go through the roller nip; otherwise, serious mechanical problems may result and recalibration will be essential. 13.2 Dry the rollers thoroughly by running them in 741 DUP050297923 # D 4361 Samples Ink Vehicles Inkometer Type mechanical electronic electronic electronic TABLE 1 Standard Deviation and Precision of Apparent Tack Readings Speed of . Rollers, r/min Standard Deviation WlthirXaboratory Between-laboratory 1 min 6 min 1 min 5 min Repeatability 1 min 5 min 800 0.49 0.47 800 0.31 0.46 400 0-38 0.37 800 0.26 0.52 0.97 0.67 1.26 1.30 1.60 1.20 2.0 1.8 1.2 1.8 1.1 1.0 0.7 Reproducibility 1 min 2.0 2.6 3.8 3.4 5 min 3.8 ~ 5.0 4.7 contact at high speed for a minimum of 5 min or until all of the solvent has evaporated. 13.3 Check the zero reading as in 12.2. Continue cleaning and drying until the dry reading reaches 0 0.5 g-m. 13.4 When the rollers are satisfactorily clean, stop the Inkometer and disengage the measuring and vibrator rollers. 13.5 Clean the pipet, the ink knife, and the glass plate with a solvent-wet rag. 14. Report 14.1 Report the following information; 14.1.1 Complete identification of the sample, 14.1.2 Inkometer model used, 14.1.3 Test speed, 14.1.4 Ambient temperature, 14.1.5 Any modifications to this test method, 14.1.6 Whether significant flying or misting was observed, 14.1.7 Whether Inkometer squeal was noted during the test, 14.1.8 Average apparent tack reading of two determina tions, and 14.1.9 Any additional apparent tack readings determined at constant speed-constant time intervals or varying speedsconstant time intervals. 15. Precision and Bias 15.1 Precision: 15.1.1 In an interlaboratory study5 of this test method six inks with a broad range in tack were measured for apparent tack ten times at I min and 5 min on mechanical Inkometers in six laboratories and on electronic Inkometers in eight laboratories. 15.1.2 In a separate interlaboratory study6 of this test method, four quick-set vehicles and four heat-set vehicles with a broad range in tack were measured in duplicate on two different days at 1 min and 5 min at 400 r/min on electronic Inkometers in six laboratories. The four quick-s t vehicles were also measured at 1 min at 800 r/min. 15.1.3 The within-laboratory/ and between-Iaboratoi v standard deviations are shown in Tabic 1. Biased on these' standard deviations the following criteria should be used for; judging the acceptability of results at the 95 % confidence level: 15.1.3.1 Repeatability--Two individual results obtained1 by the same operator should be considered suspect if they differ by more than the values given in Table 1. 15.1.3.2 Reproducibility--Two results, each the mean of two readings, obtained by operators in different laboratones should be considered suspect if they differ by more than (he values given in Table l. 15.2 Bias--Bias cannot be determined as there are no known methods for measuring actual splitting forces. The-, are indications that apparent tack measurements from the Inkometer correlate best with transfer performance when a series of test samples is based on the same vehicle chemistry 16. Keywords 16.1 apparent tack; Inkometer; printing inks; splittin forces; tack; tackmeters; vehicles 5 Supporting data are available from ASTM Headquarters. Request RR:D011039. 6 Supporting data are available from ASTM Headquarters. Request RR:D0i 1062. % 9 742 DUP0502 97924 1 # D 4361 ANNEX (Mandatory Information) Al. INFORMATION CONCERNING INKOMETERS .1 Routine Maintenance of the Inkometer A1.1.! Routine maintenance of the Inkometer is ex|femely important to the mechanical integrity of the instru ment; see the manufacturer's current instruction manual for specific model. A 1.1.2 The measuring and vibrator rollers may acquire a ;ed or shiny appearance with use, depending on the test Item and the wash-up solvent. This glaze may result in a lificant change in the apparent tack reading of an ink or iicle. The glaze may be removed by extra cleaning with a mg solvent such as acetone. If not, the composition rollers should be replaced. 'IX;e\vl.'2 Breaking-in the Inkometer Rollers ] 1 e*,J Ai I-* he sre * he.1? at llil S"J i 4,1.2.1 New Inkometer measuring and vibrator rollers selectively absorb certain components of some test gems, up to a saturation point, at which point they may be to be broken in. Until this selective absorption is plete, tack determinations made with these rollers may |be repeatable. Break in new rollers using the following ibedure: j . Al.:.2.1.1 Place the rollers on jthe Inkometer. Choose as :ak-in samples those representative of the system that will evaluated on the rollers. Run approximately 1.0 to 1.5 mL pie break-in sample for extended periods oftime, wash-up 8Si the solvent to be used, reapply the sample, run, h-up, etc. &TE Al; I ---1The wash-up is a significant part of the break-in :S3. 1 ' HJl.2.1.2 Break-in time may vary from several hours to eral days. Reproducible apparent tack readings on fidard samples (see Al.5.1), over a period of several days, . ieate that the rolls are broken in; they may then be put routine use. Al .2.2 A major change in ink systems may adversely |qt the Inkometer rollers. When a set of rollers has been ' for one system, and it is to be.used for another, use this i;e break-in procedure. The rollers may then no longer be itable for the original system. |}3 Temperature Control of the Inkometer Water Bath U.3.1 Extremely precise temperature control of the kometer water bath is essential for repeatable apparent : readings. A 1.3.2 The thermometer furnished with the mechanical Inkometer, and the temperature gage of the electronic Iiikometer are accurate to 0.5F (0.3C). A1.3.2.1 It may be advantageous to use a Bomb Calorim eter Thermometer ASTM 56F, 66.0 to 95.00T, with divi sions of 0.05F, or ASTM 56C, 19.00 to 35.00"C, with divisions of0.02C, in the Inkometer water bath. Position the thermometer in such a manner that the bottom of the mercury bulb is in line with the return inlet from the brass roller. Al.3.3 The temperature-control system of the Inkometer is capable of controlling the temperature inside the brass roller within 0.5F (0.3C). , Al ,3.3.1 It may be advantageous, particularly, if high-tack samples are run for .extended periods of time, or if the Inkometer is in constant use, to augment the temperature control system with a cold-water cooling coil. A coiled length of '/4-in. (6.3-mm) outside-diameter copper tubing may be placed in the water-bath reservoir, in the flow area away from the thermometer. The coil is connected to a cold-water tap with a pressure regulator and emptied into a sink or drain, A1.-1 Reading the Mechanical Inkometer Balance-Beam A1.4.1 In order to take a reading from the balance beam of a mechanical Inkometer, disengage the beam and move the sliding weight until the beam is continuously in balance. Read the scale at the left of the sliding weight, using the scale alignment cutout to facilitate reading. A 1.4.2 Minimization of parallax is necessary for repeatable apparent tack readings. It may be useful to mount a small reflective surface on the beam stop behind the zero indicator and the balance b^am. The zero indicator and the zero line on the balance beam are aligned in the reflective surface when an apparent tack reading is being taken. A 1.4.3 Reengage the balance beam immediately after taking the reading. A1.5 Standard Test Samples Al.5.1 It may be useful to designate one or more inks or vehicles as standards. Samples that are stable and have a good shelf life without a change in apparent tack reading (for example, tack rated or tack graded) are appropriate. Daily apparent tack readings on these samples ensures that the Inkometer is in calibration and serves as a check on repeatability. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Yourcomments are invited either forrevision of this standardor for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration af a meeting of the responsible technical committee, v/hich you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 743 DUP0502 97925 Designation: D 4366 - 91 Standard Test Methods for Hardness of Organic Coatings by Pendulum Damping Tests1 This standard is issued under the fixed designation D 4366; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover the use of pendulum damping testers in the determination of hardness of organic coatings that have been applied to acceptably plane rigid surfaces, such as a metal or glass panel. 1.2 Two test methods based on different pendulum types are covered as follows: 1.2.1 Test Method A--Konig Pendulum Hardness Test 1.2.2 Test Method B--Persoz Pendulum Hardness Test 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels12 D 1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 3. Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 Konig hardness--time in seconds for the swing amplitude of the Konig pendulum to decrease from 6 to 3". 3.1.2 Persoz hardness--time in seconds for the swing amplitude of the Persoz pendulum to decrease from 12 to 4. 4. Summary of Test Methods 4.1 A pendulum resting on a coating surface is set into oscillation (rocking) and the time for the oscillation ampli tude to decrease by a specified amount measured. The shorter the damping time, the lower the hardness. 5. Significance and Use 5.1 The pendulum damping test has been found to have good sensitivity in detecting differences in coating hardness, where hardness is defined as resistance to deformation. 5.2 The two procedures given in these test methods embody the principle that the amplitude of oscillation of a pendulum touching a surface decreases more rapidly the softer the surface. However, these test methods differ in respect to pendulum dimensions, and period and amplitude of oscillation. 5.3 In general, the damping time of the Konig pendulum is approximately half that of the Persoz pendulum. 5.4 The Persoz pendulum has a greater degree of discrim ination than the Konig for measuring the hardness of soft coatings, but it may not be as suitable for testing hard, slippery films because of its tendency to skid on surfaces with! a low coefficient of friction. 5.5 The interaction between the pendulum and the paint film is complex, it depends on both elastic and viscoelastic - i properties, and it may not be possible to establish a precise relationship between the two types of pendulum tests. TEST METHOD A--KONIG PENDULUM HARDNESS TEST 6. Apparatus 6.1 Konig Pendulum Testerf consisting of a stand that supports a pendulum, a test panel, and a pendulum displace ment scale. The stand has a stirrup to support the pendulum above the table and a mechanism for shock-free lowering of the pendulum onto the, test panel. A typical apparatus is shown in Fig 1. N()' 1--Optional features may be the inclusion of an electronic l device for automatically tinting the oscillation damping and the inclu sion of an oscillation counter. 6.2 Konig Pendulum, consisting of an open framework connected by a cross-bar, to the underface of which are t'>. > balls, 5 0.005 mm in diameter of hardness 63 3.3 HRC. inset to serve as the fulcrum. The lower end of the frame work is formed into a pointer. A weight sliding on a vertical rod attached to the cross-bar is used to counterpoise the pendulum. The total weight of the pendulum shall be 200 0.2 g. ' 6.3 Slop Watch, or other timing device for tinting the oscillation damping of the pendulum. 6.4 Polished Plate (Float) Glass Panel, for calibrating the pendulum. 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D0L23 on Physical Properties of Applied Paint Films. Current edition approved Sept. 15, 1991. Published November 1991. Originally published as D 4366 - 84. Last previous edition D 4366 - 87. 2 Annual Book ofASTM Standards, Vol 06.01. -`Pendulum hardness testers meeting the apparatus requirements of this test method may be obtained from BVK-Gardner, Inc., 2435 Linden Lane, Silver Spring, MD 20910, Paul N. Gardner Co., Inc., 316 N.E. First Street, P.O. Box 10688, Pompano Beach, FL 33061-6688 and Zorelco Limited, P.O. Box 25500, Cleveland, OH 44125. 744 DU P05 02 97926 D 4366 swing to decrease from 6 to 3 falls within 250 10 s (corresponding with 172 to 185 pendulum swings). 8. Test Panel Preparation and Conditioning 8.1 Apply uniform coatings of the materia! to be tested to plane, rigid surfaces, such as metal or glass panels, by one of the procedures given in Test Methods D 823. 8.2 Cure the coated panels under the conditions of humidity and temperature, as agreed upon between the purchaser and seller. 8.3 Measure the thickness of the dry coating in accor dance with Test Methods D 1005, D 1186, or D 1400. N*+' 2--Coating thickness must be controlled closely because the pendulum test results can be affected by thickness variations. A minimum thickness of 25 pm is required to minimize substrate effects. FIG. 1 Apparatus alibration Jjl Check the alignment of the pendulum and panel table "Hows. 1.1 Place the polished glass panel on the panel table and bring the pendulum to rest on the surface of the glass. 1 te the pendulum oscillates freely. Jji.2 Place a spirit level bn the glass panel surface. Level Jlass panel by means ofthe adjusting screws'at the base of 'instrument. .13 Clean the glass panel by wiping with a soft, lintless wetted with the solvent mixture specified in Practice '1. |T.4 Clean the fulcrum balls by wiping with a soft tissue "id with solvent. Leave the pendulum in ambient condi" and then bring it to rest on the glass panel, f.5 Check the position of the scale relative to the ulum pointer. With the pendulum at rest, its pointer ;'d indicate zero on the scale. If the pointer does not ate zero, move the scale to obtain the correct zero :ig. Check the duration of the pendulum swing on the panel. i,l Deflect the pendulum through 6, release it and ultaneously start a stopwatch or other timing device. 2.2 Determine whether the time for 100 swings of the .. ulum falls within 140 2 s. |2.3 If the measured time is less than specified, move the i|ht on the pendulum rod upward. If the measured time is ie than specified, move the weight downward. Continue J|istments until the specified time is obtained. If the time [not be obtained, the instrument should be judged faulty 1 be repaired. 3 Check the duration of damping of the pendulum on glass panel as follows: ,3.1 Deflect the pendulum through 6, release it and iultaneously start the stopwatch or other timing device. 1.3.2 Determine whether the time for the amplitude of 9. Procedure 9.1 Unless otherwise specified, make the hardness deter mination at 73.5 3.5F (23 2C) and 50 5 % relative humidity, after holding the test panels under these condi tions for at least 16 h. 9.2 Place the test panel on the panel table and gently bring the pendulum onto the panel surface. 9.3 Deflect the pendulum through 6, release it and simultaneously start the stopwatch or other timing device. 9.4 Determine the time for the amplitude of swing to decrease from 6 to 3. This is the Konig hardness. 9.5 Repeat steps 9.2 through 9,4 on at least two other areas of the test panel. 10. Report 10.1 Report the following information: 10.1.1 Mean and range of the Konig hardness values in seconds obtained for the test panel, 10.1.2 Manufacturer and model of the hardness tester used, 10.1.3 Mean and range of tite thickness values obtained for the coating on the test panel, and the method used for determining the thickness, 10.1.4 Temperature and relative humidity during the test, and 10.1.5 Test panel preparation and conditioning tech niques used. 11. Precision4 11.1 Method A--Konig Pendulum Test--On the basis of an interlaboratory test of this test method in which operators in four laboratories made three hardness measurements on each of six coated panels covering a wide range of hardness on two days, the within-laboratory coefficient of variation was found to be 3 % with 24 df and the between-laboratories coefficient of variation 8 % with 18 df. Based on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level. 11.1.1 Repeatability--Two results, each the mean of three determinations on a specimen, obtained by the same oper- 4 Supporting data are available from ASTM Headquarters. Request RR: DOM050. 745 DUP050297927 < j ;i, ! D 4366 ator should be considered suspect if they differ by more than 8 % of their mean value. 11.1.2 Reproducibility--Two results, each the mean of three determinations on a specimen, obtained by operators in different laboratories should be considered suspect if they differ by more than 23 % of their mean value. TEST METHOD B--PERSOZ PENDULUM HARDNESS TEST 12. Apparatus 12.1 Persoz Hardness Tester,4 consisting of a stand that supports a pendulum, a test panel, and a pendulum displace ment scale. The stand has a stirrup to support the pendulum above the table and a mechanism for shock-free lowering of the pendulum onto the test panel. A typical apparatus is similar to that shown in Fig. 1. 12.2 Persoz Pendulum, consisting of an open framework connected by a cross-bar, to the underface of which are two stainless steel balls, 8 0.005 mm in diameter of hardness 59 HRC, inset to form a fulcrum. 12.2.1 Pointer, attached to the lower end of the frame work, the tip of which shall be 400 0.2 mm below the plane of the fulcrum. The total weight of the pendulum shall be 500 0.1 g. 13. Calibration 13.1 Check the alignment of the pendulum and panel table. 13.1.1 Follow the procedures outlined in 7.1.1 to 7.1.4. 13.2 Check the duration of the pendulum swing on the glass panel. 13.2.1 Deflect the pendulum through 12, release it and simultaneously start the stopwatch or other timing device. 13.2.2 Determine whether the time for 100 swings of the pendulum falls within 100 0.1 s. 13.2.3 If this value cannot be achieved, reclean the glass panel and the bearing balls of the pendulum, recheck the level of the glass panel, and retest. It is not permissible to adjust the instrument scale at this point. 13.3 Check the duration of damping of the pendulum on the glass panel as follows: 13.3.1 Deflect the pendulum through 12, release it and simultaneously start the stopwatch or other timing device. 13.3.2 Determine whether the time for the amplitude of swing to decrease from 12 to 4 falls within 400 10 s. 13.3.3 If this value cannot be achieved, repeat the glass panel and instrument checks described in 13.2.3. 14. Procedure 14.1 Unless otherwise specified, make the hardness deter. mination at 23 2C and 50 5 % relative humidity, after holding the test panels under these conditions for at least ]( h. 0 14.2 Place the test panel on the panel table and gently bring the pendulum onto the panel surface. 14.3 Deflect the pendulum through 12, release it, and simultaneously start the stopwatch or other timing device. 14.4 Determine the time for the amplitude of swing t0 decrease from 12 to 4. This is the Persoz hardness. 14.5 Repeat steps 14.2 to 14.4 on at least two other areas of the test panel. ^J f; *; || \ !? J; f> > I 15. Report 15.1 Report the following information: 15.1.1 Mean and range of the Persoz hardness values in seconds obtained for the test panel, 15.1.2 Manufacturer and model of hardness tester used, 15.1.3 Mean and range of the thickness values obtained for the coating on the test panel, and the method used for determining the thickness, 15.1.4 Temperature and relative humidity during the test, and 15.1.5 Test panel preparation and conditioning tech niques used. 1i 16. Precision4 16.1 Method B--Persoz Pendulum Test--On the basis of an interlaboratory test of this test method in which operatois 1 \f 1 ii; in five laboratories made two or three hardness measure i \ ments on each of six coated panels (covering a wide range of hardness), the within-laboratory coefficient of variation was 'r t found to be 1 % with 24 df and the between-laboratories coefficient of variation 3 % with 12 df. Based on these 4* coefficients, the following criteria should be used for judging, the acceptability of results at the 95 % confidence level. 16.1.1 Repeatability--Two results, each the mean ofthree determinations on a specimen, obtained by the same oper ator should be considered suspect if they differ by more than 3 % of their mean value. 16.1.2 Reproducibility--Two results, each the mean of three determinations on a specimen, obtained by operators in different laboratories should be considered suspect if they differ by more than 8 % of their mean value. 17. Keywords i 17.1 damping hardness tests; Konig pendulum hardness 3 > tester, organic coatings; pendulum hardness tests; Persoz pendulum hardness tester The American Society lor Testing and Materials fades no position respecting the validity of any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement ofsuch rights, are entirely their own responsibility. This standard Is subject to revision at any time by tfre responsible technical committee and must be reviewed every five years and Itnot revised, eitherreapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 flace St., Philadelphia, PA 19103. 746 DUP050297928 # Designation: D 4370 - 84 (Reapproved 1990)e1 less deterdity, after it least 16 nd gently se it, and ; device. ' swing to 5. ther areas values in ter used, obtained i used for g the test, ing tech ie basis of operators measuree range of ation was boratories on these ir judging level. .n of three une opernore than nean of perators tif they hardness ts; Persoz Standard Test Methods for Acid and Base Milliequivalent Content of Electrocoat Bath1 This standard is issued under the fixed designation D 4370, the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (*) indicates an editorial change since the last revision or reapproval ei N,-' --Editorial changes were made throughout in May 1990. 1. Scope 1.1 These test methods cover the determination of acid aod base milliequivalent contents of anodic and cathodic electrocoat baths and their ultrafiltrates. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Document 2.1 ASTM Standard: D1193 Specification For Reagent Water2 3. Summary of Test Methods 3.1 Specimens are titrated with standard acid and alkali solutions respectively. Alternative procedures are given for determining acid and base concentrations potentiometrically or using a pH meter. 4. Significance and Use grades may be used, provided it is ascertained that the reagent is of sufficiently high purity to permit its use without lessening the. accuracy of the determination. 6.2 Purity of Water--References to water shall be under stood to mean water conforming to Type II of Specification D 1193. 6.3 Potassium Hydroxide Solution in Methanol, 0.1 N-- Prepare by dissolving 5.6 g of potassium hydroxide (KOH) pellets in 1 L of methanol. Standardize against NIST standard reference material of add potassium phthalate No. 84 using an automatic potentiometric titrator4 to a given end point or, alternatively, to a phenolphthalein end point. 6.4 Hydrochloric Acid Solution, 0.1 A--Prepare by mixing about 8.50 mL of concentrated hydrochloric acid (HCI) (1.19 sp gr) into a mixture of 600 mL water and 400 mL methanol. Standardize against 0.1 N potassium hy droxide solution (see 6.3). 6.5 1,3-Propanediol (Propylene Glycol) (PG). 6.6 Tetrahydrofuran (THF). 6.7 Reference pH Standard Solutions--Commercial standards of pH 4.0, 7.0, and 10.0. 4.1 The acid and base concentrations are a measurement of the titratable acidic and alkaline components in the electrocoat baths. These measurements are used for research, production or electrocoat bath process control. 5. Apparatus 5.1 Automatic Potentiometric Titrator with Stirrer and Recorder, any model. 5.2 Analytical Balance, with sensitivity of 0.1 mg. 5.3 pH Meter, any model. 5.4 Glass and Saturated Calomel Electrodes. 5.5 Syringes, 5-mL disposable. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shaft be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chem ical Society, where such specifications are available.3 Other 7. Sampling and Sample Preparation 7.1 The sample should be obtained while the electrocoat bath is under proper circulation such that a uniform material is obtained. In case of an ultrafiltrate, the material should be thoroughly mixed or stirred prior to sampling to assure uniformity. 7.2 After sampling and prior to removing a test specimen, it is mandatory that the samples be shaken or stirred until they are homogeneous and free of any settled material. This is particularly important if there is a delay between sampling the bath and performing the test. The absence of settled material can be ascertained visually (in a transparent con tainer) or by inserting a spatula, scraping the bottom of the container, and making sure that there is no settled matter. The shaking or stirring of the samples should be carried out up to the moment of taking a specimen; this Point is Very Important. 8. Base Concentration Content 8.1 Stir the sample very thoroughly to disperse materials 1 These test methods are under the jurisdiction of ASTM Committee D-I on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paint and Paint Materials. that might have settled to the bottom of the container. With the aid of a syringe, withdraw approximately 5 mL of the Current edition approved June 28, 1984. Published November 1984. 2 Annual Book ofASTM Standards, Vols 06.03 and 11,01. ...................... 3 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by ! the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York. NYihd the "United States Pharmacopeia." 4 Svelila, G., Automatic Potentiometric Titration. Pergamon Press, 1978, p. 187. 747' DUP050297929 D 4370 sample quickly, weigh the full syringe to 0.1 mg, and record this weight as W7,. Transfer the entire contents of the syringe into a 100-mL beaker. Reweigh the empty syringe to 0.1 mg and record as W2. Duplicate the procedure using a second specimen. 8.2 Add approximately 40 mL of THF/PG 80/20 mixture to the specimens in the beakers and cover, preferably with aluminum foil, to minimize evaporation of the solvent mixture. N./' I--In cases where the recommended THF/PG 80/20 mixture causes precipitation of the material, substitute the same amount of an appropriate solvent or solvent mixture to a new specimen The formation of a precipitate during the titration might foul the electrode system and mask potentiometric changes. Other solvents suitable for dilution are acetone, dimethylformamide, toluene, or methafiol. Any other solvent or solvent mixture that does no: cause the formation of a precipitate throughout the titration is suitable. In certain instances it may be necessary to run a titration blank and to make the appropriate corrections for the solvent. 8.3 Titrate both specimens with 0.1 N HC1 s'olution using the automatic potentiometric titrator until aii end point "break" is reached.4 Add approximately 5 mL of additional titrant to complete the curve. A typical titration curve is shown in Fig. 1. Record as K, the volume of titrant needed for the end point. (a) Acid Mliliequivalent Content Titration FIG. 1 (b) Base Milliequivalent Content Titration Potentiometric Titration Curves for the Acid and Base Milliequivalent Content N01' 2--Ifthe titration curve does not show an inflection point (end point), back titration with 0.1 ArKOH will give an acceptable result. 9. Base Content Calculation 9.1 Calculate the base content as folldws: A - (V, x (W, A',) x 100 - W2)M where: A = milliequivalents of base per gram of nonvolatile matter, = volume of HC1 titrant used, mL, JV, = normality of HC1 titrant, W, = mass of the syringe filled with sample, mg, w2 = mass of the empty syringe after delivery of the specimen, mg, and M = nonvolatile matter content, % . 10. Acid Concentration Content 10.1 Using a fresh portion of the sample, follow 8.1 and 8.2. 10.2 Titrate both specimens with 0.1 N KOH solution using the automatic potentiometric titrator until an end point break is reached. Add about 5 mL more of titrant ti complete the curve. From the curve, determine and record as V2, the volume of titrant needed for the end point.4 11. Acid Content Calculation 11.1 Calculate the acid content as follows: . (V2xN2)xl00 A-(W^wW where: A = milliequivalents of acid per gram of nonvolatile matter, V2 = volume of KOH titrant used, mL, N2 = normality of KOH titrant, W2 -- mass of the syringe filled with sample, mg, = mass of the empty syringe after delivery of the specimen, mg, and M = nonvolatile matter content, %. 12. Base Concentration Content Using a pH Meter 12.1 Proceed in accordance with 8.1 and 8.2. 12.2 Standardize the pH meter at 4.0 and 7.0. 12.3 Titrate both specimens with 0.1 N HC1 until a pH-of... 4.0 is obtained. Make certain that the solutions are well agitated during titration (a magnetic stirrer is recom-,i mended). Record volume of titrant, as Vs, used for titration. Because eiectrocoating paints vary greatly, it might" be advisable to titrate to a pH value agreed upon between the prdducer and the user, 13. Base Content Calculation 13.1 Calculate the base content as described in Section 9. 14. Add Concentration Content Using a pH Meter 14.1 Proceed in accordance with 8.1 and 8.2. 14.2 Standardize the pH meter at 7.0 and 10.0. 14.3 Titrate both specimens with 0.1 N KOH until a pH ? of 10.0 is obtained. Make certain that solutions are well;* agitated during titration (a magnetic stirrer is recom mended). Record volume of titrant, as V2 used for each. 748 DUP050297930 4cid Content Calculation 15.1 Calculate the acid content as described in Section 11. Precision '6.1 In an interlaboratory study of the test methods, in eh six laboratories measured in duplicate on two days electrocoat samples with acid and base milliequivalents ng from 0.2 to 0.8, the within-laboratory coefficient of ion, after discarding one,result, was found to be 1.4 % ve at 23 df and the between-laboratory coefficient of ion 5.7 % relative at 19 df. Based on these coefficients, the following criteria should be used for judging the accept ability of results at the 95 % confidence level: 16.1.1 Repeatability--Two results, each the mean of du plicate determination, obtained by the same operator on different days should be considered suspect if they differ by more than 4.1 % relative. 16.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 17 % relative. 17. Keywords 17.1 acid content; base content; electrocoat baths The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of die validity of any such patent rights, and the risk of infringement of such rights, are entirely theirown responsibility. This standard is subfect to revision at any time by the responsible technical committee and. must be reviewed every five years end if not revised, either reapproved or withdrawn. Y,curcomments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive carefui consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should mate your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 749 DUP050297931 Designation: D 4399 - 90 Standard Test Method for Measuring Electrical Conductivity of Electrocoat Baths1 This standard is issued under the fixed designation D 4399; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the electrical conductivity of electrocoat baths or ultrafiltrate samples using commercially available equipment. 1.2 This standard does not purport td address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine-the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D1125 Test Methods for Electrical Conductivity and Resistivity of Water2 D 1193 Specification for Reagent Water3 3. Summary of Test Method 3.1 A specimen is placed in a conductivity cell, or conversely a conductivity cell is placed in an eiectrocoat material, and the cell is connected to a conductivity bridge. The electrical conductivity is read directly off the meter of the bridge as the instantaneous peak reading. 4. Significance and Use 4.1 The conductivity of eiectrocoat baths results from the presence of ionic species in the bath, which come from the vehicle and from the presence of impurities present as ionizable acids, bases, salts, or combinations of these. The presence of excessive amounts of ionic impurities is detri mental to the application and performance properties of electrocoating paints. The test is suitable for use in research, production, quality control and eiectrocoat bath process control. 4.2 Other related methods for determining the electrical conductivity of water are described in Test Methods D 1125. 5. Apparatus 5.1 Conductivity Bridge- -Battery, or AC/DC line-oper- ated, capable of. providing a conductivity reading almost instantaneously. 5.2 Conductivity Cell--Dip or fill type, cell constant of 1.0. 1 This test method is under the jurisdiction of ASTM Committee D-l on Pamt and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.2! on Chemical Analysis of Paint and Paint Materials. Current edition approved May 25. 1990. Published July 1990. Originally published as D 4399 - 84. Last previous edition D 4399 - 85a, 2 Annual Book ofASTM Standards, Vol 11.01. 3 Annual Book ofASTM Standards, Vois 06.03 and 11.01. 5.3 Thermometer--Any type capable of 0.5C accuracy with a --2 to 32C range. 5.4 Measuring Vessel--Any suitable cylindrical contain.,, capable of holding sufficient eiectrocoat sample to cover th electrodes of the conductivity cell, and allowing at least 25 mm between the conductivity cell and the sides of the vessel 6. Reagents and Materials 6.1 Purity of Water--References to water shall be understood to mean water conforming to Type II of Specification D 1193. 6.2 Cleaning Solvent--An appropriate solvent for the eiectrocoat material under measurement. 7. Sampling and Sample Preparation 7.1 The sample should be obtained while the eiectrocoat bath is under proper circulation so that a uniform sample obtained. In the case of an ultrafiltrate, the material should be thoroughly mixed or stirred prior to sampling to ensure uniformity. 7.2 After sampling and prior to removing a test specimen, it is mandatory that the samples be shaken or stirred until they are homogeneous and free of any settled material. This is particularly important if there is a delay between sampling," the bath and performing the test on the bath materials. lh;1 absence of settled material can be ascertained visually ( transparent container) or by inserting a spatula, scraping the ` bottom of the container and making sure that there is i ( settled matter. Shake or stir the sample until specimens are , taken for measurement; THIS POINT IS VERY IMPORTANT. 8. Procedure 8.1 Calibrate the conductivity cell prior to use followk the manufacturer's instructions. 8.2 Rinse the measuring container several times with portions of the eiectrocoat material under test. 8.3 Take a representative portion of the eiectrocoat bath or permeate sample and place it in the measuring contain * Stir the specimen thoroughly to keep it from settling. 8.4 Adjust the temperature of the specimen to 25 0.5"( This is very important, since temperature differences cause disagreements in results and are a major source of error in these measurements. 8.5 Immerse the cell in the specimen, and move the cel1 up and down several times to displace any air bubbles from inside the cell. Hold the cell in a slightly inclined position in the center of the container with the vents at the top ofthe cell housing beneath the surface of the liquid. If a fill-type cell is used, pour the specimen into the conductivity cell. 8.6 Read and record the conductivity as described in the 750 DUP050297932 iracy the ufacturer's instructions regarding the use of the instrupnt. Avoid measuring times longer than 15 s to prevent ctrocoat sample deposition on the cell electrodes. Perform xmd measurement on another specimen, repeating steps 3 and 8.6. Calculate the mean of both measurements. 7 Take extreme care to prevent contamination of the pie and equipment. Rinse the cell with deionized water an appropriate solvent immediately after use. Keep cell ~.n and do not allow the dry electrocoat sample to ; rmulate on the interior of the cell. i. Report >1 Report the conductivity in terms of microsiemens (or |jpcroohrns per centimetre) to the nearest 1 % of the deter mined conductivity. fJO Precision and Bias I^slO.l Precision--In an interlaboratory study of this test ethod, with five laboratories measuring five electrocoat bath samples with conductivities ranging from 720 to 1750 pS/cm (microohms/cm), the intralaboratory coefficient of variation was found to be 2.6 % relative at,25 df, and the in terlaboratory coefficient of variation 4.2 % relative at 20 df. Based on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % con fidence level: 10.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 7.6 % relative. 10.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 16.5 % relative. 10.2 Bias--No bias has been determined for this test method. 11. Keywords 11.1 electioconductivity; electrocoat bath The American Society for Testing and Materials takes no position respecting the validity of,any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revfejon at any time by the responsible technical committee and must be reviewed every five years and ifnotrevised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of tho responsible technical committee, which you may attend, if you feel that your comments have hot received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 5 i to? 751 I DUP050297933 Designation: D 4400 - 89a Standard Test Method for Sag Resistance of Faints Using a Multinotch Applicator1 This standard is issued under the fixed designation D 4400; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<?) indicates an editorial change since the last revision or reapproval. N23' --Paragraph 9.3.1,1 was editorially corrected and the year date was changed Oct. 6. 1989. INTRODUCTION The multinotch applicator used in this test method is a drawdown blade with a series of notches of successively higher clearance, referred to as the Anti-Sag Meter. See Figs. 1 and 2 for a representative diagram and photograph. The numerical value for sag resistance obtained with this instrument is referred to as the Anti-Sag Index. Anti-Sag Meters are made with several clearance ranges for different types of coatings (see 5.1). In developing this test method the task group used ah instrument with a range from 4 to 24 mils, but this test method is applicable to any clearance range, and results using instruments with overlapping ranges correlate and have equal validity. This test method covers two procedures. Procedure A was developed in 19622,3 and is referenced in U.S. Federal specifications TT-E-508, TT-E-506, and TT-P-15I1. Procedure B is a newer method that obviates concern about the effect of substrate wetting as a possible variable. Numerical values obtained with the two procedures are not necessarily equal, but their rank orders are essentially the same. A preshear program is essential for a drawdown sag test to duplicate the breakdown in structure that occurs when thixotropic paints are applied by brushout or other practical application methods. The procedures therefore include the preshearing of paints just prior to making test applications. 1. Scope 1.1 This test method covers the laboratory determination of the sag resistance of aqueous and nonaqueous liquid coatings at any level of sag resistance. 1.2 Procedure A is applicable to coatings of any type or color. 1.3 Procedure B is applicable to any type of coating but does not work well with dark colors. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: ' This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D0I.42 on Architectural Finishes. Current edition approved Oct- 6, 1989. Published December 1989. Originally published as D 4400 - 84. Last previous edition D 4400 - 89. 2 "Design ofan Improved Sag Tester," Official Digest, Vol 34, No. 453, October 1962. 3 "Thixotropy... Trade Sales Paints." Official Digest, Vol 36, No. 468, January 1964. D2196 Test Methods for Rheological Properties NonNewtonian Materials by Rotational (Brookfiil Viscometer1 2 3 D 3980 Practice for Interlaboratory Testing of Paint 4>> Related Materials4 2.2 U.S. Federal Standards:5 Federal Test Method Standard 141, Method No. 494, Sa Test (Multinotch Blade) 2.3 U.S. Federal Specifications:5 Fed. Spec. TT-E-508 Alkyd semi-gloss enamel Fed. Spec. TT-E-506 Alkyd gloss enamel Fed. Spec. TT-P-1511 Interior latex gloss and sen-i-gbv. finishes !1 3. Summary of Test Method 3.1 Procedure A, Horizontal Stripes--After preshean the coating is applied to a test chart with a multim applicator. The charts are immediately hung vertically < the drawdown stripes horizontal, similar to rungs of a 11 k' with the thinnest stripe at the top. After drying in position, the drawdown is examined and rated for saggini typical sag pattern obtained by this procedure is show! Fig. 3. 3.2 Procedure B, Vertical Stripes--Two straight lires ** A Annual Book ofASTM Standards, Vol 06.01. 5 Available from Standardization Documents Order Desk, Bldg. 4, Seclio 700 Robbins Avc., Philadelphia. PA 19111-5094. 752 DUP050297934 # D 4400 FIG. 2 Medium Range Anti-Sag Meter i n\ n mross a test chart using a suitable marker pen. After r u-shc.ii ng, the coating is applied with a multinotch appli- um si' that the stripes are perpendicular to the lines. After airing briefly for the marker ink to migrate through the wet 7m, the charts are hung vertically with the stripes vertical, milar to the slats of a picket fence, with the thinnest stripe the left. After drying in this position, the ink lines are [mined and rated for sagging. A typical sag pattern {Stained by this procedure is shown in Fig. 4, 'significance and Use |4.1 Evaluation of sag resistance is essential in quality ntrol for both producers and purchasers of coatings, .ucal application tests are poor in reproducibility while imetric methods, for example Test Methods D 2196, are '--'onsuming and lack the convincing aspect of actual ging. This method provides simple and rapid tests, '"-ehy sag resistance is demonstrated by a visible sag lei ii, and is rated objectively in terms of numerical values at correlate with brushout test observations. tpparatus ;5.1 Multinotch Applicator, Anti-Sag Meter6, a drawdown "Available from The Leneta Co., P.O. Box 86, Ho-Ho-Kus, NJ 07423. An i * lua r'ay be used. FIG. 3 Typical Sag ,|attern--Procedure A blade with a series of notches of successively higher clear ance. Select a clearance range suitable for the type of coating under test in accordance with Table 1. 5.2 Test Surfaces, sealed; smooth-surfaced paper test charts, with sizes and designs as follows: 5.2.1 Black and White Charts,1* about 75/s by 1 P/a in. (193 by 288 mm), the black area comprising about SVi in. (140 mm) centered on the drawdown path. A chart of this design is shown in Figs. 3 and 5. 5.2.2 Plain While Charts1 about IVs by 11'A in. (193 by 285 mm). 5.2.3 Plain White Charts1 about 5'h by 11`A in. (140 by 285 mm). The use of a chart of this description is shown in Fig. 4. 5.3 Glass Drawndown Plate, plus straightedge guide for attachment thereto. 1 The following are available from The Leneta Co.: Black and White Chans, Form 7B. Plain While Charts, 7s* by in.. Form WB. Plain White Charts, by ll'A, Form WM. Catch-Papers, Form CP-2. 753 DUP050297935 # D 4400 TABLE 1 Anti-Sag Meter Types Type of Coaling Under Test Clearance Range, mils Range Reference Architectural Industrial--OEM. High buiEd Architectural 3-12 1-6 14-60 4-24 ,, Standard Low High Medium Number Ciearanc 10 11 11 11 ,, f. ^WmSSmmSSMMSSk,::. FIG. 4 Typical Sag Pattern--Procedure B 5.4 Catch-papers,7 thin sheets of sealed paper, for catching surplus paint at the completion of a drawdown. 5.5 Fine-Line Marker. Pens--The ink "shall be a solventbased type that wets readily and dries quickly on smooth nonporous surfaces, specifically: 5.5.1 A pen8 that applies a hydrophilic ink line for use with water-dispersed coatings. 5.5.2 A pen9 that applies an oleophilic ink line for use with solvent-dispersed coatings. 5.6 Equipment for the Preshearing ofAqueous Coatings: 5.6.1 Syringe, 10-mL, Becton-Dickinson, Luer-Lok dis posable plastic type.10 11 '5.6.2 Syringe Needle, 15 g by l`/2 in. (40 mm) to fit syringe. 5.6.3 Syringe Extension Tubing, clear vinyl, inside diam eter '/s in. (3.2 mm), outside diameter % in. (5 mm), 5.7 Equipment for the Preshearing of Nonaqueous Coat ings: 5.7.1 Rotary Mechanical Stirrer, variable speed. 5.7.2 Circular Mixing Paddle," diameter approximately l7/s in. (48 mm). 5.7.3 Mixing Container, cylindrical jar or can with ca pacity of up to 1 pt (500 mL)l 6. Procedure A--Horizontal Stripes 6.1 Preparation of Sample: 8 "Vis-A-Vis" pens, manufactured by Sanford Pen Company, Bcliwood, [L 60104, have been found satisfactory. These are sold at commercial stationers. 9 A "Flow Master" refillable pen with a fine line adapter and red Flow Master ink have been found satisfactory. The pen and the ink are sold separately. Both are manufactured by Faber-Castell Pen Corp. Newark, NJ 07107, and are available at commercial stationers. 10 Luer-Lok is a trademark of Becton-Dickinson, Beaver Brook R&, Lincoln Park, NJ 07035. Available from distributors of general laboratory supplies. 11 A mixing paddle (Catalog Number PM-70) with a diameter of l7/* in. (48 mm) made by Shur-Ltne Mfg. Co., 2200 Commerce Rd., Lancaster, NY 14086 has been found satisfactory for this purpose. This or equivalent paddles may be purchased at most hardware stares. N56' --Note use of straightedge guide. FIG. 5 Drawing Down with the Anti-Sag Meter 6.1.1 Stir thoroughly with a spatula in the original con-' tainer. 6.1.2 Strain if necessaiy to remove large particles or skins 6.1.3 Adjust the temperature of the coating to 73.5 3.5T (23 2"C). 6.2 Preshearing with Syringe and Needle (Aqueous Coat ings): 6.2.1 Prepare the paint as described in 6.1. 6.2.2 Cut a 2'A-in. (60-mm) length of syringe extension tubing and attach it to the syringe. 6.2.3 Press the syringe ban-el firmly to expel air, dip the end of the syringe into^tbe coating, pump slightly to expci remaining air, then withdraw 8 mL of coating. 6.2.4 Remove and discard the extension tubing and then attach a syringe needle. 6.2.5 Eject the contents of the syringe in front of the applicator as rapidly as possible, with firm, steady pressure 6.3 Preshearing with a Rotary Mechanical Mixei (Nonaqueous Coatings): 6.3.1 Prepare the paint as described in 6.1 and fill the mixing container slightly more than half. Set the container under the stirrer so that the paddle is about Vi in. (5 mm) from the bottom. 6.3.2 Mix vigorously for 1 min at a speed sufficient form a moderate vortex, with the entire contents of the can in rapid circular motion. Rotor speeds of 1300 to 3600 r/min have been found satisfactory, the optimum speed depending;;; on the relative diameters of the mixing paddle and container, 4 For referee tests the operators should agree upon the specific;: container, paddle, and mixing speed. 6.3.3 Immediately after mixing place about 8 mL of paint; in front of the applicator and draw down in accordance witKj 6.4 (Procedure A) or 7.4 (Procedure B). 6.4 Application ofthe Test Coating- 754 DU P050297936 4.1Affix, a suitable test chart onto the drawdown plate, black and white charts in accordance with 5.2.1 for light moderately dark colored coatings and white charts in rdance with 5.2.2 for very dark coatings. .4.2 Fasten the straightedge onto the drawdown plate in 'table position. i:4.3 Place the Anti-Sag Meter at the far end of the chart, open side toward the operator and shoulder against the ightedge guide. 14.4 If desired, position a catch-paper just underneath Tower edge of the chart. .4.5 Preshear in accordance with 6.2 or 6.3 and immediy draw down the coating at a uniform speed of about 6 #150 mm)/s, with the applicator pressed against the ghtedge to maintain a straight path. See Fig. 5 for ^ration of this step. 6.4.6 Immediately hang the chart with the drawdown 5es in a horizontal position like rungs in a standing 'er, the thinnest stripe at the top, and allow to dry in that jtion. A typical test pattern derived using this procedure is Jyn in Fig. 3. js5. Rating-the Drawdown: jS.l When the film is dry, note the notch numbers Iked on the Anti-Sag Meter and identify the correjiding stripes accordingly. $5.2 Observe the sag pattern, ignoring the bottom stripe, ~h serves only as a position reference for the stripe above and the leading and trailing edges of the drawdown, 'dering only the central 5'/' in. (140 mm) of the blade This corresponds to the black area of the black and `e chart described in 5.2.1. (See Fig. 3 for a typical sag em of this typed .5.3 Select the lowest (thickest) stripe that has resisted 'ing the gap to touch the next lower stripe. This is 'red to as the index stripe. " A Estimate the degree to which the next lower stripe ipost-index stripe) has merged with the one below it, and rmine the corresponding addendum fraction, as specified 'Table 2. ,5.5 Multiply the fraction from 6.5.4 by the difference rifecn the index and post-index stripe number to obtain index addendum. >5.6 Add the index addendum to the index stripe her to obtain the Horizontal Anti-Sag Index and record je. Procedure B--Vertical Stripes .1 Preparation ofSample--Follow procedure in 6.1. .2 Preshearing with Syringe and Needle (Aqueous Coat- --Follow procedure in 6.2. Preshearing with a Rotary Mechanical Mixer (Non~ous Coatings)--Follow procedure in 6.3. TABLE 2 Intermediate Ratings Degree of Merger of Post-Index Stripe Addendum Fraction Complete Almost complete Somewhat more than half Half Somewhat less than half SBght (just touching) 0.0 0.2 0.4 0.5 0.6 0.8 7.4 Application of Test Coating: 7.4.1 On a plain white test chart as described in 5.2.3, using the appropriate pen described in 5.. 5, rule two parallel lines about 116 in. (40 mm) apart, across the intended path of the drawdown blade (see Fig. 4). If desirecl the operator can prepare a supply of such charts for future use, since the ink line is unaffected by aging.12 7.4.2 Affix the ruled test chart onto the drawdown plate and fasten the straightedge in suitable position. 7.4.3 Place the Anti-Sag Meter at the top of the chart, the open side toward the operator and shoulder against the straightedge guide. 7.4.4 If desired, position a catch-paper just underneath the lower edge of the chart. 7.4.5 Preshear in accordance with 6.2 or 6.3 and immedi ately draw down the coating at a uniform speed of about 6 in. (150 mm)/s, with one arm ofthe applicator pressed gently against the straightedge to maintain a straight path. This procedure is the same as that referred to in 6.4 and illustrated in Fig. 5. 7.4.6 Fifteen seconds after completing the drawdown, hang the chart with the stripes vertical (like fence pickets), thinnest stripe to the left, and allow to dry in that position. A typical test pattern obtained using this procedure is shown in Fig. 4. 7.5 Rating the Drawdown: 7.5.1 When the film is dry, note the notch numbers marked on the Anti-Sag Meter and identify the corre sponding stripes and sag loops accordingly. 7.5.2 Examine Fig. 6 and note the "reference loop," which was selected because it indicates a limited but unambiguous sag movement. By actual measurement this loop represents '/u in. (1.5 mm) of sagging, which amount can be considered as defining the reference loop. 7.5.3 For each of the two ink lines on the test drawdown, note the loop that shows the same or almost as much sag as the reference loop. This is referred to as the "index" loop. The loop to its immediate light is the "post-index" loop and the corresponding stripes are the "index" and "post-index" stripes. 7.5.4 Estimate the visual difference between the index and reference loops as a fraction (to the nearest fifth or half) of the difference between the index and post-index loops. This is the addendum fraction, permissible values being 0, 0.2, 0.4, 0.5, 0.6, or 0.8. 7.5.5 Multiply the addendum fraction from 7.5.4 by the difference between the index and post-index stripes to obtain the index addendum. 7.5.6 For each ink line, add the index addendum to the index strip'e number to obtain the Vertical Anti-Sag Index and record the mean value. 8. Report 8.1 Report the following information: 8.1.1 Procedure A--The Horizontal Anti-Sag (HASI) of the coating as recorded in 6.5.6. 8.1.2 Procedure B: Index u Charts with suitable ink lines are available from The Leneta Co. Refer to Form WM-BL (Blue Line) and Form WM-RL (Red Line) for hydrophilic and oleophilic ink lines respectively. 755 DU P050297937 D 4400 $ /k ft N78' --The "reference loop" is 1.5 mm (Vie in.) deep. FIG. 6 Sag Loops Obtained with Procedure B 8.1.2.1 The Vertical Anti-Sag Index (VAS1) of the coating as recorded in 7.5.6. 9. Precision13 9.1 Correlation--In an interlaboratory study in which operators in seven laboratories tested six water-reducible paints covering a wide range of sag resistance and in five laboratories tested four solvent-reducible paints covering a wide range of sag resistance, the Spearman Rank Correlation Coefficient was 0.92 for Procedure A and 0.96 for Procedure B versus brushouts (a coefficient of 1.0 indicates perfect agreement in ranking). 9.2 Sensitivity--In the interlaboratory study described in 9.1, the sensitivity criterion values have been computed to be 4 for brushouts, 11 for Procedure A, and 13 for Procedure B. 13 Supporting dala are available from ASTM Headquarters. Request RR: DO 1-1040. Thus, Procedures A and B are approximately three tin more sensitive to differences in sag resistance than brushouts 9.3 Precision: 9.3.1 Two interlaboratory tests were conducted to est; lish the precision of this test method. The first test was tl described in 9.1. The second test consisted of operators m five laboratories performing three tests on each of thiee paints. On the basis of the second interlaboratory test, ihe within-laboratory pooled coefficients of variations for both water- and solvent-reducible paints were 4.4 % for Procedure A and 5.0 % for Procedure B. On the basis of the first interlaboratory test, the between-laboratory pooled coefiicient ofvariation for Procedure A was found to be 12.4 % for water-reducible paints and 8.8 % for solvent-reducible paints. The between-laboratory pooled coefficient of-varia tion for Procedure B was found to be 8.0 % for waterreducible paints and 6.6 % for solvent-reducible paints, Based on these coefficients of variation, the following critena should be used for judging the acceptability of results at ihe | 95 % confidence level: 9.3.1.1 Repeatability--Two results obtained by the same operator for either water-reducible or solvent-reducible paints should be considered suspect if they differ by more than 10.7 % using Procedure A and by more than 13.6 using Procedure B. 9.3.1.2 Reproducibility--Two results obtained by opera tors in different laboratories using Procedure A should be suspect if they differ by more than 34.4% for v.jii, reducible paints and 23.4 % for solvent-reducible paints. Two results obtained by operators in different laboratories using Procedure B should be suspect if they differ by more' than 23. i % for water-reducible paints and 19.8 % for solvent-reducible paints. 10. Keywords 10.1 Anti-Sag Index; rheological properties; sag-resistance The American Society tor Testing arid Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determinatiomof the validity ot any such patent rights, and the risk of infringement ot such rights, are entirety their own responsibility. This standard is subject to revision af any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 756 DUP0502 97938 Designation: D 4414 - 84 (Reapproved 1990)ei ree times rushouts to estab Standard Practice for was tha raters ii Measurement of Wet Film Thickness by Notch Gages1 of threetest, tin for both This standard is issued under the fixed designation D 4414; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 'rocedtm the first (> N9:' --Sections 5 through 10 were editorially renumbered in May 1990. d coeffi. 14 % f0l reducible of variair waters : paints, g criteria Its at thi he same' educible by more . 13.6% , Scope . pl.l This practice describes the use of thin rigid metal ptched' gages, also called step or comb gages;' in the Measurement of wet film thickness of organic coatings, such i paint, varnish, and lacquer. |il.2 Notched-gage measuremepts are neither accurate nor fisitive, blit they are useful in determining approximate wet Sn thickness of coatings on articles where size(s) and ape(s) prohibit the use of the more precise methods-given Methods D 1212. 1.3 This practice is divided into the following two proce- mined to lie between the clearance of the shortest tab wet by the film and the clearance of the next shorter tab not wetted by the film. 3.3 Procedure B--A circular thin rigid metal gage having spaced notches of varying depths around its periphery is rolled perpendicularly across the film. After removal from the film, the gage is examined and the film thickness is ' determined as being between the clearance of the deepest face wetted and the clearance of the next deepest notch face not wetted by the film. y operal iOUld be- res; 1.3.1 Procedure A--A square or rectangular rigid metal ige with notched sides is used to measure wet filhi V.JGCI- ftknesses ranging from 0.5 to 80 mils (13 to 2000 pm). i paints, 11 ' brich a gage is applicable to coatings on flat substrates and to iratories * " Sitings on articles of various riles and complex shapes )y more I# iere it is possible to get the end tabs of the gage to rest in i % : for t he same plane on the substrate. 1.3.2 Procedure B--A circular thin rigid1 metal notched f '.ge is used to measure wet film thicknesses ranging from 1 Jivv 100 mils (25 to 2500 pm). Such a gage is applicable to sistaijisej t t latings on flat substrates and to coatings on objects of * irious sizes and complex shapes. ] % 1.4 This standard does not purport to address the safety * 'oblems associated with its use. It is the responsibility of ver uses this standard to consult and establish appro- e dafety and health practices and determine the.appltca- of regulatory limitations prior to use: 4. Significance and Use 4.1 Wet film thickness measurements of coatings applied on articles can be very helpful in controlling the thickness of the final dry coating, although in some specifications the wet film thickness is specified. Most protective and high perform ance coatings are applied to meet a requirement or specifica tion for dry film thickness for each coat or for the completed coating system, or for both. 4.2 There is a direct relationship between dry film thick ness and wet film thickness. The wet film/dry film ratio is determined by the volume of volatiles in the coating as applied, including permitted thinning. With some flat coat ings the dry film thickness is higher than that calculated from the wet film thickness. Consequently, the results from the notch gage are not to be used to verify the nonvolatile content of a coating. 4.3 Measurement of wet film thickness at the time of application is most appropriate as it permits correction and B| Referenced Document 12.1 ASTM Standard: ID 1212 Methods for Measurement of Wet Film Thickness j of Organic Coatings2 adjustment of the film by. the applicator at the time of application. Correction of the film after it has dried or chemically cured requires costly extra labor time, may lead to contamination ofthe film, and may introduce problems of adhesion and integrity of the coating system. Summary of Practice 4.4 The procedures using notched gages do not provide as accurate or sensitive measurements of wet film thickness as 3.1 The material is applied to the articles to be coated and do the fnterchemical. and Pfund gages described in Methods |le wet film thickness measured with a notched gage. D 1212. Notch gages may, however, be used on nonuniform 13.2 Procedure A--A square or rectangular thin rigid metal surfaces, like concrete block, that are too rough to use the j||ge with notched sides, having tabs of varying lengths, is Interchemical and Pfund gages. Also notched gages can be Bfished perpendicularly into the film. After removal from the very useful in the shop and field for determining the Rim, the gage is examined and the film thickness is deter- approximate thickness of wet films over commercial articles where size(s) and shape(s) are not suitable for measurements by other types of gages. Examples of such items are ellipses, This practice is under the jurisdiction of ASTM Committee D-1 on Paint and ted Coatings and Materials and is the direct responsibility of Subcommittee 01.23 on Physical Properties of Applied Paint Films. Current edition approved Oct. 26, 1984. Published January 1985. 2 Annual Bonk ofASTM Standards, Vol 06.01. thin edges, and corners. 4.5 An operator experienced in the use of a notched gage can monitor the coating application well enough to ensure the minimum required film thickness will be obtained. 757 DU P0502 97939 D 4414 4.6 Application losses, such as overspray, loss on transfer, and coating residue in application equipment, are a signifi cant unmeasurable part of the coating used on a job and are not accounted for by measurement of wet film thickness. 5. Report 5.1 Report the following information: 5.1.1 The mean and range of the readings taken and the number of readings. 5.1.2 The smallest graduation of the gage used. 6. Precision and Bias 6.1 The precision and bias of Procedure A or B for measuring wet film thickness with notch gages are very dependent on methods of film application, time that the measurement is taken after film application, mechanical condition of the notch gages, and the step range of the gages. 6.2 Generally, the agreement between notch gages is good because they are insensitive to small differences in film thickness, that is the step intervals of the gages are relatively large. PROCEDURE A 7. Apparatus 7.1 Notched Gage, square or rectangular, thin rigid metal plate, with notched sides (see Fig. 1), made from steel or aluminum3 (Note 1). Nonmetallic gages shall not be used. N;<' 1--Aluminum or aluminum alloy gages'are more easily distorted and may exhibit greater wear than steel gages. Gages made of plastic or deformable metal are not suitable. 7.1.1 Each notched side shall consist of a series of tabs (between notches) varying in length and located in a line between two end tabs equal in length and longest in the row. 7.1.2 As an example, the tabs on one row of a gage may differ in length as follows: By 0.5 mil (13 pm) between 0 and 6 mils (0 to 150 pm). By 1 mil (25 pm) between 6 and 10 mils (150 to 250 pm), By 2 mils (50 pm) between .10 and 30 mils (250 to 750 pm), and By 5 mils (125 pm) over 30 mils (750 pm). 8. Procedure 8. i Apply the coating material to a rigid substrate and test with the gage immediately. The gage must be used immedi ately following application of the coating, Some coatings lose solvents quickly and spray application increases the speed. The resulting rapid reduction in wet film thickness can cause misleading readings. 8.2 Locate an area sufficiently large to permit both end tabs of the gage to rest on the substrate in the same' plane. 8.3 Push the gage perpendicularly into the wet film so that the two end tabs rest firmly on the Substrate at the same time. 8.4 Or, set one end tab firmly on the substrate and lower the gage until the other end tab is firmly in contact with the substrate. 8.5 Remove the gage from the film and examine the tabs. * These gages are commercially available from various coating equipment and instrument suppliers. (--vrtna- trtnnnj-ur P | 6' a/ (9o) oc o"Tc "1 > tt> 19 70 77 LyUT-A_A. 18 FIG. 1 Rectangular Notched Gage The film thickness is determined as being between the clearance of the shortest tab wetted and. the clearance of the next shorter tab not wetted by the film. 8.6 Clean the gage immediately after each reading by wiping it on a dry or solvent-dampened cloth so that subsequent readings are not affected. Do not clean with metal scrapers. 8.7 Repeat the procedure in 8.2 through 8.5 for at least three locations on the film. The number of readings required to obtain a good estimate of the film thickness varies with the shape and size of the article being coated, with the operator's experience, and whether one or more of the following problems are encountered: 8.7.1 Some coatings may not wet (leave residue or metal gages. However, the film itself may show when: contact was made. When reading the gage, look at both the. gage and the film itself for verification of the reading. 8.7.2 The gage may slip on the surface. Ignore such read ings. 8.7.3 The surface may be coarse and false readings pro duced. The spot where the gage is used must be as unik i m possible and questionable readings ignored. 8.8 Determine the mean and range of the readings. PROCEDURE B 9. Apparatus / 9.1 Circular Notched Gage, thin aluminum disk, with notches of various depths spaced around its periphery (see Fig. 2). Each notch has a recessed flat face. A Ys-in. (10-mtn) hole is in the center of the disk. 4 758 DUPO 502 97940 Designation: D 4417 - 84 Standard Test Methods for Field Measurement of Surface Profile of Blast Cleaned Steel1 1. Scope 1.1 These test methods cover the description of tech niques for measuring the profile of abrasive blast cleaned surfaces in the laboratory, field, or in the fabricating shop. There are additional techniques suitable for laboratory use not covered by these test methods. 1.2 This standard may involve hazardous materials, oper ations. and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability ofregulatory limitations prior to use. 2. Summary of Method 2.1 The methods are: 2.1.1 Method A--The blasted surface is visually compared to standards prepared with various surface profile depths and the mode determined. 2.1.2 Method B--The depth of profile is measured using a fine pointed probe at a number of locations and the arithmetic mean determined. 2.1.3 Method C--A composite plastic tape is impressed into the blast cleaned surface forming a reverse image of the profile, and the peak to valley height on the tape measured with a micrometer. 3. Significance and Use 3.1 The height of surface profile has been shown to be a factor in the performance of various coatings applied to steel. For this reason, surface profile should be measured prior to coating application to ensure that it meets the specification. The instruments described are readily portable and suffi ciently sturdy for use in the field. N=>' --Optical microscope methods serve as a referee method for surface profile measurement. Profile depth designations are based on the concept of average maximum profile (7r max); this value is determined by averaging a given number (usually 20) of the highest peak to lowest valley measurements made in the field of view of a standard measuring microscope. This is done because of evidence that coatings performance in any one small area is primarily influenced by the highest surface features in that area and not by the average roughness.12 4. Apparatus 4.1 Method A--A profile comparator3 consisting of a number of areas (each approximately one square inch in size), usually side by side, with a different profile or anchor 1 These lest methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D0I.46 on Industrial Protective Painting. Current edition approved Nov. 14, 1984. Published January 1985. 2 John D. Keane, Joseph A. Bruno, Jr.. Raymond E. F. Weaver, "Surface Profile for Anti-Corrosion Paints," Oct. 25, 1976. Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, PA 15213. 3 Suitable comparators include Keane-Tator Surface Profile Comparator and Clemtex coupons. pattern depth. Each area is marked giving the nominal profile depth in mils or micrometres. Typical comparator surfaces are prepared with steel shot, steel grit, or sand or other nonmetallic abrasive, since the appearance of the profile created by these abrasives may differ. The comparator areas are used with or without magnification of 5 to lOx. 4.2 Method B--A dial gage4 depth micrometer fitted with a pointed probe. The probe is machined at a 60" angle v..ih, nominal radius of 50 pm. The base of the instrument rests on the tops of the peaks of the surface profile while the spring loaded tip projects into the valleys. 4.3 MethodC--k special tape containing a compressible foam attached to a noncompressible uniform plastic film. A burnishing tool is used to impress the foam face of the i.t, . into the surface to create a reverse replica of the profile that is measured using a spring-loaded micrometer.5 m 5. Test Specimens 5.1 Use any metal surface that, after blast cleaning, is free ofloose surface interference material, dirt, dust, and abi isiu residue. 6. Procedure 6.1 Method A: 6.1.1 Select the comparator standard appropriate for the abrasive used for blast cleaning. 6.1.2 Place the comparator standard directly on the sur face to be measured and compare the roughness of the prepared surface with the roughness on the comparator segments. This can be done with the unaided eye, under 5 to lOx magnification, or by touch. When using magnification, the magnifier should be brought into intimate contact with the standard, and the depth of focus must be sufficient so that the standard and surface are in focus simultaneously. 6.1.3 Select the comparator segment that most closely approximates the roughness of the surface being eval 1 it-c or, if necessary, the two segments to which it is intermediate. 6.1.4 Evaluate the roughness at a sufficient number of locations to characterize the surface as specified or agreed upon between the interested parties. At each location make three evaluations against the comparator and determine the mode. The mode of the three evaluations represents the profile at the specific location, with the mode of all locations representing the profile of the entire surface. 6.2 Method B: 6.2.1 Prior to use set the gage to zero by placing it on a piece of plate glass. Hold the gage by its base and press firmly against the glass. Adjust the instrument to zero. 6.2.2 To take readings, hold the gage firmly against the prepared substrate. Do not drag the instrument across the try 4 Suitable depth micrometers include the Elcometcr Model 123 Surface Prrfilc Gage. 5 Suitable replica tape and micrometers include Testex "Prcss-O-l-ilm" tape and Mitutoyo Model 7326 Spring Micrometer. 760 DUPO 502 97942 D 4417 ninal trator id or f the rator x. with itha resit. 'ring able n. A I ape at is free:;',:; iive!i"ti | (face between readings, otherwise the spring-loaded tip ay become rounded. 6.2.3 Measure the profile at a sufficient number of locaas to characterize the surface, as specified or agreed upon tween the interested parties. At each location make ten ^readings and determine the mean. Then determine the mean ' all the locations and report it as the profile of the surface, h. n.3 Method C: *'' ,0.3.1 Select the correct tape range for the profile to be asured: coarse, 0 to 2 mils (0 to 50 pm) and extra coarse, i to 4.5 mils (40 to 115 pm). |.3.2 Remove the wax paper backing and place the tape .off the prepared surface with the foam side down, that is, put tilie dull side down. 6.3.3 Hold the tape firmly on the surface and rub the jfeular cut-out portion (approximately % in. (6.5 mm) meter) with the burnishing tool until a uniform gray color ears. jj|,3.4 Remove the tape and place it between the anvils of a ring-loaded micrometer. Measure the thickness of the tape (compressed foam and non-compressible plastic film com bined). Subtract the thickness of the noncompressibie plastic film to obtain the surface profile. 6.3.5 Measure the profile at a sufficient number of loca tions to characterize the surface, as specified or agreed upon between the interested parties. At each location make three readings and determine the mean. Then determine the mean for all the locations and report it as the profile of the surface. 7. Report 7.1 Report the range and the appropriate average (mean or mode) of the determinations, the number of locations measured, and the approximate total area covered. 8. Precision 8.1 Precision is under active study.6 6 Other organizations, such as National Association of Corrosion Engineer (NACE), are currently involved in suefi studies. The American Society tor Testing and Materials takes no position respecting the validity of any patentrights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard Is subject to revision atany time by the responsive technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invitedeither torrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, tf you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. the arhe :or to 3 Er'J. a" s .3 761 DUP050297943 (JOT9 Designation: D 4449 - 90 Standard Test Method for Visual Evaluation of Gloss Differences Between Surfaces of Similar Appearance1 This standard is issued under the fixed designation D 4449; the number immediately following the designation indicates the year of original adaption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or rcapprovui. 1. Scope 1.1 This method covers the visual evaluation of gloss differences of coating surfaces, using special types of lamps for illumination. It identifies six aspects or types of gloss that one may look for when using the lamp to assess gloss differences between surfaces. It describes the conditions for using the lamps to best identify small differences in each of the six types of gloss. Four levels of visual gloss differences are distinguished. 1.2 While this technique is useful for both weathered and unweathered specimens, it has not been applied to mctallics. 1.3 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information only. 1.4 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D3964 Practice for Selection of Coating Specimens for Appearance Measurements13 * E 284 Definitions of Terms Relating to Appearance of Materials3 3. Terminology 3.1 Definitions--For definitions of terms used in this method, see Definitions E 284. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 directionality ofsurface--perceived change of glossy appearance of a surface with rotation of the surface in its own plane (see Fig. 1). 3.2.2 gloss, distinctness-of-image--perceived sharpness of images reflected by an object surface (see Fig. 2). 3.2.3 gloss, ofa surface--perceived directionally selective reflecting properties responsible for the degree to which reflected highlights or images of objects may be seen as superimposed on the surface. 3.2.4 reflection haze--cloudy or milky appearance of a 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.26 on Optical Properties. Current edition approved Oct. 26, 1990. Published December 1990. Originally published as D4449 - 85. Last previous edition D 4449 - 85. Annual Book of ASTM Standards, Vol 06.01. 3 Annua! Book ofASTM Standards, Vol (4.02. surface adjacent to directions of specular reflection (see Ft 3). 3.2.5 sheen--perceived shininess at a near-grazing an(<f of incidence for an otherwise matte specimen (difficult i photograph). 3.2.6 specular gloss--the relative luminous refle. factor of a specimen in the specular direction. The luminou reflectance factor is the ratio of the luminous flux refle from, to that incident on, a specimen for specified soli angles (see Fig. 4), 3.2.7 texture--perceived structure, pattern, or topograj or combination thereof, of a surface (see Fig. 5). 4. Summary of Test Method 4.1 Test specimens are illuminated by special light soun that provide reflected images suitable for rating the gloss t coating surfaces. Two types of lamps may be used to produ6 reflected images. Lamp A consists of a modified fluoresceni desk lamp covered with screen mesh. Lamp B consists ofaij incandescent bare filament bulb installed in an adjustall angle fixture. 4.2 Light from the selected lamp illuminates thi specimens. The reflected images reveal specular gloss ref, tion; the sharpness of the images of the screen or Ian filament reveals the detail and quality of the surface tion (distinctness of image); and spreading of the ref light into dark areas? such as the space between fluoicsc^ tubes or near the filament image, reveals the presencsllj near-specular haze. 5. Significance and Use 5.1 Gloss4 is associated with the capacity of a surface 1 reflect more light in some directions than in others, directions associated with mirror (or specular) refleclic normally have the highest reflectances. Gloss is best seen aril analyzed when the surfaces studied are illuminated by a 1. source that provides strong contrasting patterns of light f dark. Such a light source is described in this test method. 5.2 The simplest concept of gloss is that it corresponds! the mirror-like reflectances of surfaces. However, the < butions and intensities of this surface-reflected light are (fi real materials) highly variable and affected by a variety i factors: surface smoothness and contour, refractive ind absorptance, angle of incidence, and (to a generally sn extent) wavelength. From the great variety of surface; 4 For a more detailed account of gloss, its measurement, and relationship Ugj appearance generally, see R. S. Hunter. The Measurement of Appearance, Wilfijt' Interscience New York, NY 1975. 762 DU PO 502 97944 # D 4449 N?@' --The left panel is free of directionality. The right panel, is bighly directional because of buffing marks. FIG. 1 Reflection of Bright Incandescent Lamp in Two Panels -The panels exhibit a difference In dlstinctness-of-refleoted image. FIG. 2 Two White Porcelain Enamel Panels gji election patterns met in materials of commerce, it has been jgssible to identify seven surface-reflection criteria or "types jljlloss" regularly used by skilled technologists for intercomIping and rating their products for gloss. Six of the seven fiteria, or "types of gloss," are identified in the section on . el nitions. The seventh, luster or contrast gloss, is seldom of concern to the coatings industry. 6. Apparatus 6.1 Lamp A--The recommended apparatus is constructed by modifying a conventional fluorescent desk lamp that has two I5-W, 18-in. (450-mm) tubes. Figure 6 is a photograph; 763 DU PO 5 02 97945 DU P050297946 D 4449 tfor a or tg .ru si 'a nfegn j the theja WSS; tis" m to cm. FIG. 5 Two Painted Panels Differing in Texture NAB' --The lamp is modified by the addition of a black reflecting surface behind tubes and a wire screen in front. FIG. 7 Desk Lamp -The lamp is used to demonstrate gloss or geometric differences in the arances of surfaces. FIG. 6 Modified Desk Lamp Identify differences between each pair of surfaces compared as either: Nunc (or indistinguishable) 0 Very slight (barely distinguishable) = I Moderate (easily seen) =2 Considerable =3 9.1.4 Which of the pair appears glossier (except in first case). 765 DUPO50297947 # D 4449 vr ' " , (a) For high specular gloss, distirichisss-of-image gloss, aid reflection haze (b) For intermediate and low specular gloss and directionality of plane surfaces (c) For sheen FIG. 8 Recommended Positions of Gloss Inspection Lamp, Observer, and Surfaces of Different Levels of Gloss Being lntercompar--il 10. Precision NCD' --The precision study has not been completed. 10.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than two in ratings. 10.2 Reproducibility--Two results, each the mean of two runs, obtained by operators in different laboratories t be considered suspect if they differ by more than 2.2 iti'S ratings. 1 11. Keywords i 11.1 distinctness of images; gloss; haze; visual gloss The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are express// advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely thefr own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments areinvited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible teohnicai committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP0502 97948 Designation: D 4451 - 85 {Reapproved 1991)E1 Standard Test Method for Pigment Content of Paints by Low-Temperature Ashing1 This standard is issued under the fixed designation D 4451; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reappraval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. I NEF' --Keywords were added editorially in July 1991. `M ppe ical Society, where such specifications are available.4 A;,!--.! This test method covers the pigment content ofpaints 8If ni several traffic marking materials (thermoplastic and vformed tape) by low-temperature furnace ashing. Some inic pigments may be lost by this method and some water fmoisture contained in pigments will be lost. 5.2 Toluene. 6. Procedure 6.1 Liquid-Paint: 6.1.1 Mix the sample until homogeneous, preferably on a mechanical shaker. If air bubbles become entrapped in the T This standard does not purport to address all of the paint, stir it by hand. Ifeiy problems, if any, associated with its use. It is the 6.1.2 Draw sligljtly more than 10 g.ofthe paint under test Sfafroonsibility ofthe user ofthis standard to establish appro- into a 10-mL syringe and weigh to 0.1 mg. Transfer about 5 ' ui'c safety and health practices and determine the applica- mL toluene to a porcelain dish tared with a paper clip for use mRiyeofefrreengcueldatDooryculimmeitnattsions prior to use. as a stirrer. Add 10 g of the material into the toluene. Reweigh the syringe to 0.1 mg and calculate the specimen ASTM Standards: 3723 Test Method for Pigment Content of WaterEmulsion Paints by Low-Temperature Ashing2 180 Practice for Determining the Precision of ASTM (Methods for Analysis and Testing of Industrial 1. Chemicals3 weight. Mix well on a magnetic stirrer. Place the dish in the oven at 105G for 30 min. 6.1.3 Remove and heat at the lowest temperature possible over a meker burner in a fume hood. Do not leave the dish on the burner after the flame has subsided. Transfer to the muffle furnace and proceed as in 6.4. 6.2 Preformed Traffic Marking Tape--Cut about a 10-g Summary of Test Method square of the product. Remove the adhesive by pulling it off or by using an appropriate solvent. Save the beads that are 3.1 The specimen is transferred to a tared porcelain dish, knocked off by this process and weigh with the tape. Dry the '*ed (if necessary) at 105C, and heated on a burner. The specimen for 30 min at 105"C to remove the solvent. Cool in h and specimen are transferred to a muffle furnace and a desiccator. Weigh the specimen along with the loose beads ted at 450"C. The dish and specimen are reweighed and to 0.1 mg into a tared porcelain dish. Heat in a fume hood at pigment (ash) content calculated. the lowest temperature of a meker burner in a furnace hood until the material catches fire. Do not leave the dish on the Apparatus 4-1 Muffle Furnace, maintained at 450C 25C. 4.2 Circulating Oven, maintained at 105C 2C. 4.3 Porcelain Dishes, 90-mm diameter. 1,4.4 Plastic Disposable Syringe, 10-mL capacity. #.5 Burner, meker type. burner after the flame has subsided. Transfer to the muffle furnace and proceed as in 6.4. 6.3 Thermoplastic Traffic Marking Material--This mate rial may be delivered in block or powdered form. Transfer about 400 g of the sample to a quart container and heat in a forced draft oven at 400F until completely melted (may take as long as 4 h). Stir vigorously until well mixed. Pour about 10 g of the sample into an aluminum dish and let it cool. , Reagents Remove the 10 g wafer from the aluminum dish and weigh |5.1 Purity ofReagents--Reagent grade chemicals shall be led in all tests. Unless otherwise indicated, it is intended "fit all reagents shall conform to the specifications of the ommittee on Analytical Reagents of the American Chem to 0.1 mg. Transfer to a tared porcelain dish. Heat the dish at the lowest temperature of a meker burner in a fume hood until the specimen catches fire. Do not leave the dish on the burner after the flame has subsided. Transfer to a muffle Furnace and proceed as in 6.4. 1 This test method is under thejurisdiction of ASTM Committee D-l on Paint Related Coalings and Materials and is the direct responsibility of Subcom- htee DO 1.21 on Chemical Analysis of Paints and Paint Materials. f-Curreni edition approved Jan. 25, 1985. Published December 1985. i 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 15.05. 4 "Reagent Chemicals, American Chemical Society Specifications.'' Am. Chem. Soc., Washington* DC. Por suggestions on the testing of reagents nvt listed by the American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY and the "United States Pharmacopeia." 767 i DUP050297949 D 4451 6.4 Place the porcelain dish in a muffle furnace in a fume hood at 450C (see Test Method D 3723). Heat overnight or until no further carbonaceous material is noted. Cool in a desiccator and reweigh the dish plus the residue to 0.1 mg. Calculate the residue as percent pigment or, in the case of thermoplastic material and preformed tape, as pigment and beads. 7. Calculation 7.1 Calculate the percent pigment, P, as follows: P = C-^Axioo where: C = weight of dish and specimen after ignition in furnace, g, : A = weight of dish alone, g, and S' = specimen weight used, g.` 1 8. Precision 8.1 The precision estimates are based on an interlabora tory study in which one operator in 7 different laboratories analyzed in duplicate on two days six samples of commercial whole paint or thermoplastic material containing 50 to 80 % pigment. The results were analyzed statistically in accor dance with Practice E 180 and the within-iaboratory coeffi cient of variation was found to be O.lO^ relative at 36 df and the between-laboratories coefficient of variation 0.25 % relative at 30 df. Based on these coefficients the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 8.1.1 Repeatability--Two results, each the mean of dupli cate determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 0.28 % relative. 8.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 0.72 % relative.: ft 9. Keywords 9.1 ignition, pigment; low temperature ashing; pigment content of paints the Amsticm) Society forTesting &nd Materials takes nb position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights> and the risk pf infringement of such rights,, are entirety their own responsibility, , This 'standard is subject to revision at any time by the responsible technical committee and must be reviewed every live years and if notrevised, either reapprovdd or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should he addressed to -ASTM Headquarters. Your comments will receive careiul consideration at a meeting of the responsible technical committee, which you may attend, ff you feel that your comments have not received a fair hearing you should make your views known tothe.ASTM Committee on Standards. 1916 Race St., Philadelphia, PA 19103. i i v* 768 DUP05 0297950 b Designation: D 4457 - 85 {Reapproved 1991)*1 Standard Test Method for Determination of Dichloromethane and 1,i,f-Trichloroethane in Paints and Coatings by Direct Injection into a Gas Chromatograph1 This standard is issued under the fixed designation D 4457; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. ei NGH' --Keywords were added editorially in July 1991. 8|cope ;.l This test method covers the determination of total unt of dichloromethane or 1,1,1-trichloroethane, or in paints and coatings. It has been evaluated for '{llose nitrate, alkyd, vinyl, and styrene-butadiene systems, as not yet been eyaulated for other formulations, but is eved to be applicable. The established working range of !|test method is from 31 to 65 % for 1,1,1-trichloroethane 32 to 78 % for dichloromethane. There is no reason to 'eve it will not work outside of these ranges. The presence ijrpropanol in paints and coatings requires the use of a erent internal standard. (See also Practice E 260.) |2 This standard does not purport to address all of the Jp problems, if any, associated with its use. It is the onsibility of the user of this standard to establish appro ve safety and health practices and determine the applicaj of regulatory limitations prior to use. Specific hazard raents are given in Section 7. : Referenced Documents .1 ASTM Standards: 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals2 IE 260 Practice for Packed Column Gas Chromatography3 fSummary of Test Method f.l Anhydrous 1-propanol (see 10.5) is added as an temal standard to suitable aliquot of the whole paint. The uot is then diluted with dimethylformamide and injected a gas chromatographic column containing a porous Jymer packing that separates dichloromethane and 1,1,1chloroethane from other volatile compounds. I' Significance and Use 4.1 Use of 1,1,1-trichloroethane and dichloromethane, v Inch do not measurably contribute to the atmospheric jaxidant level, is a way for industry to meet government or other regulations on volatile organic compounds. This test method is designed to determine the content of these halohydrocarbon solvents in paints and coatings. That con tent can subsequently be used in calculating the volatile organic compound content of a coating. 5. Apparatus 5.1 Chromatograph, any gas-liquid chromatographic in strument equipped with a thermal conductivity detector and capable of being temperature programmed (see Table 1). Optionally, a flame ionization detector may be used if the sample is diluted so that no more than 1000 ppm each of dichloromethane and 1,1,1-trichloroethane is present in the injected specimen. 5.2 Recorder, a recording potentiometer with a full-scale deflection of 10 mV, a full-scale response time of 2 s or less, and a maximum noise of 0.03 % of full scale. 5.3 Pre-Column, 40 in. (100 mm) long by '/in. (3.2 mm) outside diameter stainless steel, packed with glass wool, fitted on the entrance end of the column to retain any nonvolatile materials and minimize sludge buildup in the column. 5.4 Column, 4 ft (1.22 m) long by '/s in. (3.2 mm) outside diameter stainless steel, packed with 80/100 mesh (150 to 180 pm) porous polymer packing material,4 5or other suitable material. 5.5 Liquid Charging Devices, such as microsyringes of 5-pL or 10-pL capacity, cleaned with acetone or other suitable solvent. Visually inspect for plugs or cracks before and after each injection. 5.6 Vials, 25-mL to minimize head space, capable of being septum sealed.3 6. Reagents and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests, unless otherwise specified (as in 6.7). Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analyt ical Reagents of the American Chemical Society, where such specifications are available.6 Other grades may be used Hiis test method is under the jurisdiction of ASTM Committee D-l on Paint ind Related Coatings and Materials and is the direct responsibility of Subcotn- ittee D01.21 on Chemical Analysis of Paint and Paint Materials. Current edition approved July 16, 1985. Published October 1985. * Annual Book ofASTM Standards* Vol 15.05. Annual Book ofASTM Standards, Vol 14.01. A Porapak R, available from Waters Associates. Inc., Milford. MA. has been found satisfactory for this purpose. 5 Mininert valves, available from The Pierce Chemical Co., Box 117. Rockford, II. 6 H05, have been found satisfactory for this purpose. 6 "Reagent Chemicals, American Chemical Society Specifications," Am. Chem. Sou., Washington, DC. For suggestions on the testing of reagents not listed by the 769 n. DUP0502 97951  D 4457 provided it is first ascertained that the reagent is of sufficient high purity to permit its use without lessening the accuracy of the determination. 6.2 Carrier Gas, helium of 99.995 % or higher purity. High purity nitrogen may also be used. 6.3 Dimethylformamide (DMF), reagent grade. 6.4 1-Propanol, gas chromatography spectrophotometric quality (see 10.5). 6.5 1,1,1-Trichloroethane (see 6.7). 6.6 Dichloromethane (see 6.7). 6.7 Halogenated Hydrocarbon Stabilizers--All commer cial grades of these halogenated hydrocarbons contain stabi lizers. Either obtain the same solvent used in the coating for use as the standard, or find the type and quantity of stabilizer specified for use in the solvent of interest and add the appropriate quantity to the pure solvent. 7. Hazards 7.1 Dimethylformamide is harmful if inhaled or absorbed through skin. Use only with adequate ventilation. Avoid contact with skin, eyes, and clothing. 8. Preparation of Apparatus 8.1 Column Conditioning--The packed column is in stalled in the gas chromatographic unit leaving the exit end disconnected from the detector. This will prevent any contamination of the detector with the column bleed. Set the helium flow rate at 30 mL/min if a Vs in. (3.2 mm) outside diameter column is used. Purge the column 5 to 10 min before heating. Heat the column from room temperature to 200C at 5C/min and hold this temperature for at least 12 h (overnight). At the end of this period of time, heat the column to 240C at a 5C/min rate and hold this tempera ture for several hours. The maximum temperature for this packing is 250C. Cool the column to 100C and reheat to 240C at 5C/min to observe the column bleed. Optimum conditioning of this column may take several cycles of the heating program before a good recorder baseline is achieved. Conditioning of any column other than that suggested (5.4) should be in accordance with the manufacturer's recommen dations. , 8.2 Install the column in the chromatograph and use the information in Table 1 as a guide to establish the conditions required to give the desired separation. Allow sufficient time for the instrument to reach equilibrium as indicated by a stable recorder baseline. Adjust the carrier-gas flow to a constant rate. Before each calibration and series of determi nations (or daily), condition the column at 200'C for 1 h with carrier-gas flow. 9. Calibration 9.1 Preparation of Standards--All standards, as well as samples and blanks, should be at a constant temperature. The given order of ingredient addition should be observed to minimize loss of volatile ingredients. 9.1.1 Weighing to 1.0 mg, add 16.0 g of dimethyl formamide to a vial capable of being septum sealed. Add 2.0 American Chemical Society, see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United States Pharmacopeia." TABLE 1 Typical Instrument Conditions Detector Column Temperature, C Injection port Detector block Column Initial Final C/min Carrier gas Flow rate, mL/min Specimen size, pL thermal conductivity " 1 ft (1.22 m) by '/a in. (3.2 mm) outsii diameter packed with 80-100 mesh porous polymer packing 200 250 100 230 (for 8 min) 8 helium 30 1 g of 1,1,1-trichloroethane, 2.0 g of 1-propanol (see 10.5) and 2.0 g of dichloromethane. Seal the vial with a crimp-on oi septum seal. 9.2 Determine the retention time of each component by / injecting small amounts either separately or in known " mixtures. The components should elute close to the typical* retention times given in Table 1 and the chromatograms should closely approximate those shown in Fig. 1. 9.3 The area under each peak of the chromatogram is,*' considered a quantitative measure of the corresponding compound. The relative area is proportional to concentration if the detector responds equally to all the sam'ple ^ components. The response to different components is geneiU| ally significantly different for both flame ionization aml; thermal conductivity detectors and especially for ionization detectors. This difference in detector response' may be corrected by use of relative response factors obtained11 by injecting and measuring the response of known blen , For precise and accurate determination of the halogenatoi fl U-, ll <c) IV) FIG. 1 Typical Chromatograms of Paints 770 DUP050297952 D 4457 Irocarbons inject a 1 11L specimen of the standard in |ordance with the preparation in 9.1. Calculate the reSb'inse factors relative to unity for the halogenated hydrocar-:'Sfi[IS v.g- j Procedure we to. 1 Keep all samples, blanks, and standards at a constant Hgmperature. Observe the given order of ingredient addition | fo minimize loss of volatile ingredients. Shake paints, then < , Simple from the middle of the container. ('.,10.2 Weighing to 1.0 mg, add 16.0 g of dimethylfSSmamide and 5.0 g of the paint to a vial capable of being BBfijuin sealed. Add 2.0 g of 1-propanol (see 10.5). Seal the 1 IB?' w`t*1 a crtmP"on or septum seal. J Wm 10.3 Shake the vial. Then to facilitate settling, centrifuge i. a ow speed centrifuge at 1000 rpm for 5 min. ' 10.4 Inject a 1-pL specimen of the supernatant from the : "Sjjepaicd solution onto the chromatographic column, in ccordance with the conditions established in 8.2. Record fepeaks of all components. 116.5 If the composition of the paint is unknown, test for Bipresence of 1-propanol. Prepare a blank, omitting the 2.0 Ibf 1-propanol in 10.2, and inject a l-|iL specimen. To this Rpk add 2.0 g of 1-propanol and inject a 1-p.L specimen. fi|n compare peak response to that from the test solution. If fgtopanol is present in the paint, substitute a different "$ liglhial standard. Other possible internal standards include jj^iphols, esters, and hydrocarbons. *'gD,6 If the composition of the paint is unknown, establish ether peaks interfering with 1 -propanol or the halogenated Erocarbons are present by using both the column specified 1115.4 and a second column that yields different retention ><es.7 jf|. Calculation Jlfl.l Measure the area of all peaks (Note) and multiply Mph area by the appropriate attentuation factor to express -lipvpeak areas on a common basis. j. kare--Peak areas may be determined by any method that meets the jjffireasion requirements of Section 12. Electronic integration is recomSekded for best results. W1.2 Calculate the percent halogenated hydrocarbon in |g paint as follows: RFi = --W-, A - corrected peak response for i!h component, area units, = weight of i`h component in the standard solution, g, and = chromatographic peak area for the i,h component in the standard solution, area units, CH wt1 RFcn x Ac,, x ISaml RFis *A,sx IV ' Packings from the Porapak scries and the Chromosorb Century series may be jfaetory for this purpose. However, it is the responsibility of each analyst to for interferences from paints or the internal standard chosen, or both, and to : a column that gives symmetrical peaks. where: CH wt` r Fc h isam! RF,s W = chlorinated hydrocarbon, weight %, = response factor for the chlorinated hydro carbon in the standard solution, area units, = area of the chlorinated hydrocarbon peak in the test solution, area units, = weight of internal standard added to the paint, & = response factor for the internal standard in the standard solution, area units, = area of the internal standard peak in the test solution, area units, and = specimen weight, g. 12. Precision and Bias8 (see also Practice E180) 12.1 Precision: 12.1.1 J,1,1-Trichloroethane--On the basis of an inter laboratory test of this test method in which one operator in each of eight laboratories tested three coatings containing from 31 to 65% 1,1,1-trichloroethane (theoretical), the within-laboratory coefficient of variation was found to be 1.01 % relative at 20 degrees of freedom and the betweenlaboratories coefficient of variation was found to be 2.72 % relative at 17 degrees of freedom. Based on these coefficients, the following criteria should be used for judging the accept ability of results at the 95 % confidence level: 12.1.1.1 Repeatability--Two results, each the mean of duplicate runs, obtained by the same operator should be considered suspect if they differ by more than 3.0 % relative. 12.1.1.2 Reproducibility--Two results, each the mean of duplicate runs, obtained by operators in different laborato ries should be considered suspect if they differ by more than 8.1 % relative. 12.1.2 Dickloromethane--On the basis of an inter laboratory test of this test method in which one operator in each of eight laboratories tested two coatings containing from 32 to 78 % dichloromethane (theoretical), the withinlaboratory coefficient of variation was found to be 0.98 % relative at 14 degrees of freedom and the between-laboratories coefficient of variation was found to be 5.16 % relative at 12 degrees of freedom. Based on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 12.1.2.1 Repeatability--Two results, each the mean of duplicate runs, obtained by same operator should be consid ered suspect if they differ by more than 3.0 % relative. 12.1.2.2 Reproducibility--Two results, each the mean of duplicate runs, obtained by operators in different laborato ries should be considered suspect if they differ by more than 17.92 % relative. 12.2 Bias--Determination of a bias statement for this test method is not practical at this time. 33. Keywords 13.1 chlorinated hydrocarbons in paints by gas chromatograph; dichloromethane, in paints; exempted sol vent in paints; gas chromatograph, halohydrocarbon; 1,1,1trichloroethane, in paints9 9 Supporting data are available from A$TM Headquarters. Request RR:D01 1045. 771 DU P050297953 # D 4457 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feei that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia. PA 19103. 772 DUPO 50297954 F. Designation: D 4518 - 91 Standard Test Methods for Measuring Static Friction of Coating Surfaces1 is: This standard is issued under the fixed designation D 45IS; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon {) indicates an editorial change since the last revision or reapproval. l. Scope 1.1 These test methods cover the determination of the ` i sistance to sliding on coating surfaces by measuring the itatic friction. 1.2 Two test methods are described as follows: Sections ethod A--Inclined Plane Test...................................................... 8 to 13 Method B--Horizontal Pull Test.................................................... 14 to 19 'f 1.3 This standard does not purport to address all of the it ' afety problems, if any, associated with its use. It is the i esponsibility ofthe user ofthis standard to establish appro- Mate safety and health practices and determine the applicaff.- i'ility ofregulatory limitations prior to use. - Referenced Document 2.1 ASTM Standard: : D 823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 ii Terminology 3.1 Definition: 3.1.1 static friction--the force required to start the test fjjed moving, divided by the mass of the sled. ft Summary of Test Methods 4.1 With the inclined plane test (Test Method A), a jweighted sled is placed on a test specimen and the specimen fs gradually inclined from the horizontal until the sled begins t slide. The tangent ofthis angle of inclination is reported as lie static friction. ' 4.2 With the horizontal pull test (Test Method B), a ighted sled is placed on a horizontal test specimen and is pulled across the specimen. The static friction is reported as Ihe force required to start the sled moving, divided by the mass of the sled. 5. Significance and Use 5:1 The friction characteristics of coating surfaces can be important to the use of the coatings. For example, low friction of exterior can coatings is beneficial to the flow of the cans on production lines. Also low friction of interior pipeline coatings is beneficial to the flow of materials 1 These lest methods are under the jurisdiction of ASTM Committee D-l on HPpint and Related Coatings and Materials and are the direct responsibility of iSubcommittcc DO 1.23 on Physical Properties of Applied Paint Films. Current edition approved Sept. 15,1991. Published November 1991. Originally, published as D 4518 ~ 85. LaSt previous edition D 4518 - 90. 2 Annual Book ofASTM Standards, Vol 06.01. through pipes. On the other hand, low friction of floor coatings can be hazardous to foot traffic. 5.2 Under some conditions, measurement of the static friction can be used to evaluate the slip resistance ofcoatings under use conditions. However, results can be extremely dependent on the type of coating surface and the type of sliding unit used. 5.3 The tendency for footwear to slip may be influenced by foreign materials or lubricants on the shoe materials or on the walking surfaces. Also, these test methods do not incorporate all the directional forces involved in the walking process. Consequently, levels of slip resistance as determined by these test methods may not predict a person's resistance to slipping when walking on various surfaces. 5.4 The best precision and sensitivity are obtained when stainless steel is used as the facing of the sliding unit. In some tests where a leather facing is used, poor precision is obtained because of the inability to control the uniformity of its surface during the test. The use of a hard synthetic robber facing provides somewhat better precision. 5.5 These test methods provide for static friction measure ments when the sled facing and the coating surfaces are wet with water. Results from such tests must be treated with caution because frequently the static friction values obtained for wet, smooth coatings are higher than those obtained for the same surfaces dry. This is because, when stationary at tire beginning of the test, the sled contact can produce a "suction cup" effect on a wet surface. Measurements performed on wet coatings with rough surfaces have been more satisfac tory. 5.6 A test procedure is offered that eliminates the "suction cup" effect of wet surfaces. The wet sled is dropped onto the wet coating surface at the start of the test. 5.7 Results obtained by these test methods may be ex tremely sensitive to the age of the test coating because the blooming action of additives or plasticizers is often timedependent. It may be meaningless to compare slip and frictional properties oftest coatings applied at different times unless this effect is being studied. 5.8 The measurement of static friction may be influenced by the length of time that the sled rests on the test specimen before motion is initiated. 5.9 Static friction measurements have been useful in evaluating (/) the suitability of coatings for the exterior of cans, (2) the slipperiness of floor polishes, and (i) the slip resistance characteristics of footwear on floor tiles and floor coatings. Also, static friction measurements have been useful in determining the effect of coating additives (for example waxes, silicones) on the slipperiness of coating surfaces. 773 DU PO50297955 D 4518 6. Test Specimens 6.1 Apply test coatings in accordance with Test Methods D 823 to substrates of at least 4 in. (100 mm) in width and length. The substrates may be of glass, steel, aluminum, or other appropriate material that remains smooth and plane after the test coating has been applied and cured at 73.5 3.5F (23 2'C) and 50 5 % relative humidity for 7 days, unless otherwise specified. Prepare at least two test panels for each coating. 6.2 Take care during application of the test coating to minimize entrainment of dust and particulate matter in the surface of the coating. Extreme care is required when handling the panels, even after sufficient cure. The surface should be kept free of all dust, lint, fingerprints, or any foreign matter that may change the characteristics of the surface. 7. Conditions for Testing 7.1 Test the coated test specimens under one or more of the following conditions as agreed upon by the purchaser and the seller: 7.1.1 Both sled facing and coating surfaces dry at 73.5 3.5F (23 2C). 7.1.2 Both the sled face and the coating surface wet with water containing a slight amount of wetting agent at 73.5 3.5'F (23 2C). Sea water containing a slight amount of wetting agent may be used when it is appropriate. A wetting solution consisting of 1 mL of surfactant3 added to 200 mL of water has been found to be satisfactory. 7.1.3 One or both of the above at 35.5 3.5F (2 2"C). TEST METHOD A--INCLINED PLANE TEST 8. Apparatus 8.1 Inclined Plane, having a smooth, incompressible sur face, at least 1 in. (25 mm) wider than the sliding unit and of sufficient length to allow the test sled to move by gravity at least 0.5 in. (12 mm), provided with clamps for the test specimen, and an inclinometer to indicate the angular displacement of the plane to within 0.5". NIJ' 1--A suitable apparatus is shown in Fig. 1. It may be assembled from items obtained from laboratory instrument supply houses. 8.2 Test Sleds--Alternative sleds that may be used are: 8.2.1 Stainless Rounded Edge Steel Block, with a highly polished plane lower surface 3 by 3 in. (75 by 75 mm) in area and a mass of 1.8 lb (0.82 kg) to provide a pressure of 0.2 psi (1.4 kPa) when horizontal. 8.2.2 Stainless Steel Block, with a plane lower surface of 3 by 3 in. (75 by 75 mm) and a mass of 1.8 lb (0.82 kg). Adhered to the lower surface is a `A-in. (6-mm) thick vulcanized neoprene rubber having a Shore "A" hardness of 65 5. A screw eye or other means to attach the sled to the force-measuring device is provided. 8.3 Inclinator--Means to smoothly increase the inclina tion of the plane from the horizontal through an arc of at 3 A surfactant such as Aerosol OT manufactured by American Cyanamid Co., Chemical Group, One Cyanamid Plaza, Wayne, NJ 07470, has been found suitable for this purpose. least 45' at a rate of 1.5 + 0.5'/s. NKL' 2--Procedures found suitable for smoothly increasing tie. inclination of the plane arc (J) pulling the top ofthe plane upward 9 M a motor driven dip coater and (2) pushing the top of the plane up with a laboratory jack equipped with a hand crank. 9. Preparation of Apparatus 9.1 Preparation ofSled Facing: 9.1.1 If a synthetic rubber facing is used on the test sled, it must be preconditioned by light sanding before each deter mination. 9.1.2 Place a sheet of 400A wet or dry silicon carbide abrasive paper on a flat surface. Sand the synthetic ruhl i1 facing by rubbing it gently back and forth over the paper fe tv times. Repeat at 90 to the first direction. Wipe the surface of the synthetic rubber facing with a clean, dry cloth to remo dust or loose material from the surface. 10. Procedure 10.1 Level the plane so it is horizontal when the inclinom eter reads zero. 10.2 Clamp the test specimen to the plane. Recheck the levelness of the panel in two directions (along the length f* the panel and across the panel at 90 to the first measutv.ment). 10.3 Dry Surfaces: 10.3.1 Center the sled on the test coating. Immediately commence inclining at a rate of 1.5 0.5/s. When the sled starts to move, stop the inclinometer immediately and read the angle of displacement at the moment the sled starts to move. 10.3.2 Return the plane to a level position and make two additional tests on the test specimen as described in 8.3. 10.4 For Wet Surfaces: i 0.4.1 Check levelness of plane and test panel accordi to procedures given in 10.1 and 10.2. 10.4.2 Wet the test coating surface and the sled facing with the prescribed solution. Apply the solution with a soft brush. Make certain that all surfaces are completely wet. 10.4.3 Set the plane of the angle of displacement dete - 774 sof I iStef D U PO 502 97956 ft D 4518 BLE 1 Precision Values Obtained in 1987 Round-Robin Test of Test Method D 4518 Inclined Plane Test Intralaboratory Dry Surfaces Tvpe of a** Sirface Standard Deviation Angle or Static inclination Friction Coefficient of Variation Degree of Freedom Maximum Allowable Difference Angle of Static Inclindation Friction Polished steel Abraded Steel 3.6 3.7 0.08 0.08 23% 10% 14 13 10.9 0.24 11.3 0.24 Interiaboratory p*. Type of ii' s,ed !Solished Steel Ipratied Steel Pgioprene Standard Deviation Angle of Static Inclination Friction 4.2 0.09 4.0 0.09 4.2 0.21 Coefficient of Variation 28% 20% 17% Degree of Freedom 32 32 19 Maximum Allowable Difference Angle of Static Inclination Friction 12.1 0.26 11.5 0.26 12.4 0.62 1 llPne<* fr the dry coating surface in 1Q.3.1. i, 10.4.4 From a height of Vz in. (12 mm), drop the sled onto i |-L\iic coating surface. Determine if the sled begins to slide. 2 ft 10.4.5 Change the angle of the slide, and after rewetting j'-fj.Hing and sled surfaces, repeat dropping the sled. Continue .fn this manner until the plane angle at which the sled starts I '^to slide is determined. Jl . 10.4.6 Return the plane to the initial position of 10.4.3 *i-id repeat 10.4.4 and 10.4.5. it? Calculation 1,1 Calculate the mean ofthe three measurements on the specimen. Determine the trigonometric tangent of the ah angle, which is the static friction value. 12. Report 12.1 Report the following information for the coated panels tested: 12.1.1 Temperature and humidity during curing and at the time of testing, 12.1.2 Type of facing used on the test sled, 12.1.3 Whether facing and coating surface were wet or dry, 12.1.4 Inclination angle determined for each measure ment, 12.1.5 Static friction value for each measurement, and 12.1.6 Mean static friction value for the replicate panels. 13. Precision 13.1 An interlaboratory study of Test Method A (Inclined Plane Test) in which one operator in each of four laborato ries, using sled surfaces of neoprene, polished steel and mildly abraded steel, tested the dry surfaces of eight coated panels with a wide range of slip resistance. The intralabo ratory and interlaboratory standard deviations were found to be as shown in Table 1, Based on these standard deviations, the following criteria should be used forjudging, at the 95 % confidence level, the acceptability of results: 13.1.1 Repeatability--Two results obtained by the same operator should be suspect if they differ by more than the maximum allowable difference given in Table I. 13.1.2 Reproducibility--Two results obtained by opera tors in different laboratories should be considered suspect if they differ by more than the maximum allowable difference given in Table 1. 13.2 Comparison of inclined plane results are shown in Table! TABLE 2 Comparison of Inclined Plane Results Obtained with Stationary and Dropped Sleds on Panel Surfaces Panel Sled Surface Angle of Slide, Sled Stationary Sled Dropped ,. Static Friction HSled Stationary Sled Dropped fA 1B C 'D tG H Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Steel Neoprene Dry Wet Dry Wet Dry Wet Dry Wet Dry Wet Dry Wet 12 27 20 47 17 36 20 47 20 38 25 14 12 0.21 0.21 31 0.50 0.61 14 0.25 32 0.61 25 0.35 0.46 34 . 1.07 0.68 19 0.34 26 0.49 26 0.31 0.49 41 0.73 0.86 19 0.23 26 0.56 25 0.35 0.46 34 1.07 0.68 15 0.27 29 0.56 2Q 0.35 0.35 32 0.80 0.61 19 0.34 26 0.49 22 0.46 0.39 36 0.96 0.74 13 0.23 18 0.32 775 DUP05 02 97957 # 13.3 Bias cannot be determined since there is no standard for slipperiness or slip resistance. TEST METHOD B--HORIZONTAL PULL TEST 14. Apparatus4 14.1 Test Base, a horizontal plane surface of a smooth, incompressible material (metal, wood, plate glass, or plastic) having a width at least 1 in. (25 mm) wider than the test sled (14.2) with means of leveling it in two directions. This base serves as a support for the rest of the mechanism and the test specimen. When placed on a solid support, it must be free of vibration. 14.2 Test Sleds--Alternative sleds that may be used are: 14.2.1 Stainless Steel Block, with a highly polished lower plane surface of 3 by 3 in. (75 by 75 mm) and a mass of 1.8 lb (0.82 kg) to provide a pressure of 0.2 psi (1.4 MPa) on the horizontal surface. A screw eye or other means to attach the sled to the force-measuring device is provided. 14.2:2 Steel Block, with a smooth lower surface of 3 by 3 in. (75 by 75 mm) in area and a mass of 1.8 lb (0.82 kg). Adhered to the lower surface is a Vi-in. (6-mm) thick vulcanized neoprene rubber having a Shore "A" hardness of 65 + 5. A screw eye or other means to attach the sled to the force-measuring device is provided. 14.2.3 Steel Block, having a smooth lower surface 4 by 5 in. (100 by 125 mm) in area and a thickness of 1 to 1.5 in. (25 to 40 mm). Adhered to the lower surface is vulcanized neoprene rubber haying a Shore "A" hardness of 65 5 and a thickness of '/' in. (3 mm). The total mass of the sled with the rubber facing shall be 6.0 0.5 lb (2.7 0.2 kg). 14.3 Mechanical Power Unit--Means for.moving the test sled horizontally over the test specimen or the test specimen under a fixed test sled under the following conditions: 14.3.1 For the sleds described in 14.2.1 and 14.2,2, a speed of 6.0 1.0 in./min (150 25 mm/min) shall be provided and a sled (or panel) travel of 4.in, (100 mm). 14.3.2 For the sled described in 14.2.3, a speed of .12 1 in. (300 25 mm)/min shall be provided and the sled (or panel) allowed to travel 4 in. (100 mm). 14.3.3 Force Measuring Device--Means for measuring the force to 0.01 lb (0.04 N) required to move or restrain the test sled. NNO' 3--A force gage5 that can be preset to display the highest force encountered is desirable. NPQ' 4---Figure 2 illustrates a suitable apparatus. There are various commercial instruments available but some require modification to meet the requirements of these test methods. 15. Preparation of Apparatus 15.1 Preparation ofSled Facing: 15.1.1 If a synthetic rubber facing is used on the test sled, it must be preconditioned by light sanding before each determination. 15.1.2 Place a sheet of 400A wet or dry silicon carbide abrasive paper on a plane surface. Sand the synthetic rubber facing by rubbing it gently back and forth over the paper four 4 A facing of heel material such as Neolile, with a Shore "A" hardness of 95 5 may be used if appropriate. 5 Chatilton dynamometer gages, available from Chatillon, Inc., 83-30 Kew Garden Rd., Kew Garden, NY 11415, have been found suitable for this purpose. Dial ^ Gage~*A Specimen FIG. 2 Schematics for Two Horizontal Plane instruments times. Repeat at 90" to the first direction. Wipe the surface of*<J the synthetic rubber facing with a clean, dry cloth to remove ' dust or loose material from the surface. 16. Procedure 16.1 Select the test sled and traverse the speed appropriate for the type of test desired: 16.1.1 The test sled described in 14.2.2 with a traverse speed of 6 in. (150 mm)/min is recommended if the best,,' precision of measurement on a smooth coating is desired 16.1.2 The test sled described in 14.2.2 with a traverse speed of 6 in. (150 mm)/min is recommended if it is desired to measure the resistance of a smooth coating to the slipping of a rubber shoe heel or sole. 16.1.3 The test sled described in 14.2.3 with a traverse speed of 12 in. (300 mm)/min is recommended if it is desired to measure the resistance of a rough coating to the slipping of a rubber shoe heel or sole. 16.2 Clamp the test specimen to the base. Position the,t ,t , sled and connect it to the power unit or force gage. Fasten the inelastic linkage (cable or chain) to the test sled and|j connect to the power unit or the force gage. 16.3 As soon as possible after positioning the sled, star! t the power unit, taking care to maintain tautness in them linkage as the power unit takes up the load. 16.4 Record the force required to just begin motion of the test slide; that is, the maximum force value recorded. 16.5 For the evaluation of smooth coatings, make two additional determinations on the test specimen as describee in 16.1 through 16.4. For the evaluation of rough coatings, make four additional determinations on the test specimen. 17. Calculation 17.1 Calculate the mean of the force value obtained foi the replicate determinations. 17.2 Divide the mean force by the mass of the test sled. This is the static friction value. 776 DU P050297958 "IS. Report 1 18.1 Report the following information for the coated inels tested: !< 18.1.1 Temperature and humidity during curing and I sting, 18.1.2 Whether facing and coating surfaces were dry or ' et, ' 18.1.3 Mass of test sled used, 18.1.4 Type of facing used on the test sled, ; 18.1.6 Static friction value for each coated panel, and 18.1.7 Mean static friction value for the replicate panels. 19. Precision and Bias 19.1 An interlaboratory test will be conducted to determine the precision and bias of this test method. Tests conducted by several laboratories have shown that this measuring technique has sufficient sensitivity and precision to differentiate coatings exhibiting significantly different sliding friction characteristics. 20. Keywords 20.1 coating surface slipperiness; horizontal pull slipmeter test; inclined plane; static friction The American Society for Testing andMaterials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned In this standard. Users of this standard are expressly advised that determination o! the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and tl not revised, either reapprovedor withdrawn. Your comments are invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race SL, Philadelphia, PA 19103. Is !| .uM, DU P050297959 Designation: D 4537 - 91 Standard Guide for Establishing Procedures to Qualify and Certify inspection1 Personnel for Coating Work in Nuclear Facilities1 This standard is issued under the fixed designation D 4537; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This guide delineates the requirements for develop ment of procedures for the qualification of personnel who perform inspection of coating work. These activities are accomplished to verify conformance to specified require ments for nuclear facility coatings work whose satisfactory performance is required in order not to compromise systems used to mitigate the consequences of postulated accidents. 1.2 This guide provides a uniform interpretation of the requirements in ANSI/ASME N45.2.6-1978 for the inspec tion of coating work in nuclear facilities. 1.3 This guide meets the intent of ANSI/ASME NQA-1. 1.4 It is the intent ofthis guide to provide a recommended basis for qualification, not to mandate a singular basis for all qualifications. Variations or simplifications of the qualifica tions described in this guide are appropriate for special coating work outside of safety-related areas. 1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.\ ANSI/ASME Standards: ANSI/ASME N45.2.6 Qualifications of Inspection, Exam ination, and Testing Personnel for Nuclear Power Plants2 ANSI/ASME NQA-1 Quality Assurance Program Re quirements for Nuclear Facilities.2 3. Terminology 3.1 Description of Terms Specific to This Standard 3.1.1 certification--written documentation of qualifica tion. 3.1.2 coating work inspection--a phase of quality control which, by means of examination, observation, or measure ment, determines the conformance of coating work to predetermined quality requirements. 3.1.3 qualifications--skills, training, and experience re quired for personnel to perform properly the duties and 1 This guide is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.04 on inspection. Current edition approved Aug. 15, 1991. Published October 1991. Originally published as D 4537 - 86. Last previous edition D 4537 - 86. 2 Available from American National Standards Institute. 11 W. 42nd Street. 13th Floor, New York, NY 10036. execute the responsibilities of the appropriate certification level. 3.1.4 training--the program developed to ensure that personnel receive the knowledge and skills necessary for qualification. 4. Significance and Use 4.1 The requirements of this guide apply to personnel who perform inspections of coating work during (/) fabrica tion, (2) receipt of items at the construction site, (3) construction, (4) pre-operational and startup testing, and (5) operational phases of nuclear facilities. 4.2 It is the responsibility of each organization partici pating in the project to ensure that only those personnel within their respective organizations who meet the require ments of this guide are permitted to perform inspection activities covered by this guide. 4.3 The organization(s) responsible for establishing the applicable requirements for activities covered by this guide shall be identified, and the scope of their responsibility shall1 be documented. Delegation of this responsibility to other qualified organizations is permitted and shall be docu mented. 4.4 It is the responsibility of the organization performing" these activities to specify the detailed methods and proi c dures for meeting the requirements of this guide, unless they are otherwise specified'ain the contract documents. 5. General Requirements for Inspection Personnel 5.1 Provisions shall be made for the indoctrination of i personnel as to the technical objectives of the project, Ihe' j codes and standards that are to be used, and the quality"! assurance elements that are to be employed. 5.2 The need for formal training programs shall be determined, and such training activities shall be conductTM as required to qualify personnel who perform inspectionsTM On-the-job participation shall also be included in the pi gram, with emphasis on first-hand experience gained through actual performance of inspections. 5.3 A candidate's qualifications for certification shall be initially determined by a suitable evaluation of the canm date's education, experience, training, examination results, and capability demonstration. 5.4 The job performance of coating work inspection personnel shall be reevaluated at periodic intervals not to ( exceed three years. Reevaluation shall be by evidence of, continued satisfactory performance or redetermination of' capability in accordance with 5.3. If, during this evaluation ; or at any other time, it is determined by the responsible: organization that the capabilities of an individual are not 778 DUP0502 97960 Mi k P jf+jpIB. sf u' p NUMBER: i pAR DISTANCE VISUAL ACUITY | I. Jaeger J-l letters ^ * Uncorrected, normal Corrected, normal $ -OR- 2. Alternative Method:. v gill Uncorrected, normal Corrected, normal t OLOR VISION 1. Ishihara's test chart jfc 2. Alternative Method:.. t| l Color vision test findings: (Last) # D 4537 VISION TEST RECORD Expires (First) JOB NAME: _ YES YES YES YES YES (Middle Initial) NO NO NO NO je above-named individual has Passed/Failed the vision test as specified in Section 7 of this Guide. |lS CERTIFICATION IS VALID FOR ONE YEAR FROM THE DATE OF EXAMINATION. EXAMINER:______________________________________ Type or print name followed by signature TITLE:D FIG. 1 Sample Vision Test Record cordance with the qualifications*specified for the job, that son shall be removed from that activity until the required pability has been demonstrated. i5.5 Any person who has not been actively engaged in the erformance or supervision of coating work inspection for a mod of one year shall be reevaluated in accordance with .3. ( Functional Qualifications of Inspectors f6A All physical inspection activities can be performed by ertified Level I, Level II, or Level III inspectors. |'6.2 Level I Coatings Inspector, shall be capable of the illowing: 6.2.1 Implementing and recording all inspections required fy the applicable procedures. J'6.2.2 Verifying instrument calibration. 6.2.3 Performing hold point inspections in accordance Kith the applicable procedures. 6.3 Level II Coalings Inspector, shall be capable of the Sfo [lowing: 6.3.1 Performing all of the duties and responsibilities of a Level I coatings inspector. 6.3.2 Planning and supervising inspections, initiating and reviewing inspection procedures, and evaluating the ade quacy of activities. 6.3.3 Reviewing, organizing, and approving results of inspections. 6.3.4 Monitoring the performance of and supervising the work of Level I coatings inspectors. 6.3.5 Training and verifying the qualifications of Level 1 coatings inspectors for certification. 6.3.6 Initiating changes to quality procedures. 6.3/7 Implementing the Quality Assurance Program if assigned that (authority by company policy or the Quality Assurance Program. 6.4 Level III Coatings Inspector, shall be capable of the following: 6.4.1 Carrying out all of the duties and responsibilities of a Level II coatings inspector. 6.4.2 Certifying Level I,' Level II, and other Level III coatings inspectors. 779 DU P050297961 NAME: (Last) EDUCATION: W D 4537 EDUCATION AND EXPERIENCE RECORD (First) EXPERIENCE: (Middle Initial) PROFESSIONAL DATA: I certify that the above information is accurate. SIGNED: Candidate FIG. 2 Sample Education and Experience Record DATE: 6.4.3 Responsible for evaluating the adequacy of pro grams used to train coatings inspectors. 6.4.4 Responsible for authorizing Level II coatings inspec tors to carry out training and examination duties; 6.4.5 Responsible for approving all safety-related inspec tion procedures.7 7. Physical Qualifications of Inspectors 7.1 Each inspector shall be examined annually to ensure natural or corrected near-distance visual acuity in at least one eye. The individual shall read the J-l letters on a Standard Jaeger Test Chart, or equivalent, at a distance of not less than 12 in. with one or both eyes, uncorrected or corrected. 7.2 Each candidate shall be examined for color preception using the Ishihara Test or the Farnsworth D-15 Test when being certified or recertified. If a candidate does not pass the Red/Green Sensitive Ishihara Test, the candidate may take the Farnsworth D-l 5 Test. 7.3 If a candidate does not pass the Farnsworth D-15 Test the candidate may be evaluated by a licensed medical practitioner to provide the necessary data to determine the candidate's color perception. Individuals certified after an evaluation by a licensed medical practioner may only certified to perform inspection work that is within the candidates's color perception capability. 7.4 The examinations required by 7.1 and 7.2 shall burif administered by a licensed medical practitioner or a pi familiar with the tests involved. The results of vision tesi shall be documented on a Vision Test Record (Fig. '! equivalent form). 7.5 The responsible organization shall identify any othetfj physical qualifications required to perform the assigned inspection duties. Inspectors requiring the identified physical qualifications shall have them confirmed by examinations a's intervals not to exceed one year. 8. Education, Training, and Experience Qualifications 8.1 Candidates for certification as coatings inspectors shall have sufficient education, experience, and training to ensure ' an understanding of the principles and procedures in those areas of inspection, examination, and testing activities for which they are being considered for certification. 8.2 Level I Coatings Inspectors, shall, as a minimum, meet one or more of the following requirements: 780 DUP0502 97962 FIG. 3 Sample Organization Training Record 1,2.1 High school graduation plus six months of related 'Jjrience' in equivalent inspection activities. 1 J2.2 Completion of college level work leading to ah sociate Degree or higher, plus three months of related erience in equivalent inspection activities. jR3 Level II Coatings Inspectors, shall, as a minimum, ` t one or more of the following requirements: 9 13.1 High school graduation plus one year of satisfactory rformance as a Level 1 coating inspector in the corre- |hding inspection activity. 1:3.2 High school graduation plus three years of related perience in equivalent inspection activities. |3.3 Completion of college level work leading to an rssociate Degree plus one year Of related experience in divalent inspection activities. 8.3.4 Four-year college graduation plus six months of |ted experience in equivalent inspection activities. 8.4 Level III Coatings Inspectors, shall meet one or more of the following requirements: 8.4.1 High school graduation plus six years of satisfactory performance as a Level II coatings inspector in the Corre sponding inspection activity. 8.4.2 High school graduation plus ten years of related experience in equivalent inspection activities; or high school graduation plus eight years experience in equivalent inspec tion activities, with at least two years as a Level II coatings inspector. The candidate shall have at least two years associated with nuclear facilities or sufficient training to be knowledgeable of the quality assurance requirements for nuclear coating work. 8.4.3 Completion of college level work leading to an Associate Degree and seven years of related experience in equivalent inspection activities. The candidate shall have at least two years of this experience associated with nuclear 781 DUP0502 97963 # D 4537 RECORD OF CERTIFICATION TO WHOM IT MAY CONCERN: SUBJECT: Coatings Inspector Certification, Level - REFERENCE: ASTM Standard GuideRev. _ . has complied with, and successfully passed, all of the applicable requirements of the referenced Standard Guide. EXAMINATION SCORES GENERAL PORTION _ SPECIFIC PORTION___ PRACTICAL PORTION . I certify that the above statements are correct and recommend certification as a Level _______Coatings Inspector. RECOMMENDED BY NAME: ______________ TITLE: Type or print followed by signature The above statement and recommendation have been reviewed for conformance to the requirements of the referenced Standard, and are correct. This individual is certil as Lcvd __. coatings inspector in accordance with the referenced Standard Guide. CERTIFIED BY Type or print name followed by signature (must comply with 11.3 of the Standard Guide) FIG. 4 Sample Record of Certification facilities or sufficient training to be knowledgeable of the quality assurance requirements for nuclear coating work. 8.4.4 Four-year college graduation plus five years of related experience in equivalent inspection activities. The candidate shall have at least two years of this experience associated with nuclear facilities or sufficient training to be knowledgeable of the quality assurance requirements for nuclear coating work. 8.5 Compliance with the requirements of 8.1, 8.2, 8.3, and 8.4 shall be documented on an Education and Experi ence Record (Fig. 2 or equivalent form). 8.6 Training leading to certification or recertification as a qualified coatings inspector shall be documented on an Organizational Training Record (Fig. 3 or equivalent form). 9. Examination 9.1 Each candidate for coatings inspector shall be given an iilHs examination covering the general, specific, and practi aspects of coatings inspection. The general and spi portions of the examination may be written, in the form.ofa personal interview, or a combination of both. The ex.imirvtion results shall be documented in accordance with 11.1. 9.1.1 The general portion of the examination shall cover the basic principles of quality assurance and coating work inspection. 9.1.2 The specific portion of the examination shall covet specific coating work requirements and inspection pro' dures. 9.1.3 The practical portion of the examination shall cover, the use ofcoating work inspection equipment and inspect! procedures. 9.1.4 All parts of the examination for a Level I or Level II coatings inspector shall be administered by a Level 111, 782 DUP0502 97964 # D 4537 ',, rpLings inspector or a duly authorized Level II coatings 11. Certification of Inspectors '(Tpspector. 11.1 Level I and Level II coatings inspection certifications 7 5.1.5 Examinations for a Level III coatings inspector shall are valid for a period not to exceed three years. Level III j f 1)8 administered by a certified Level III coatings inspector or coatings inspector certifications are valid for a period not to t m the responsible organization's management. exceed five years. Coatings inspectors are certified after review of the candidate's qualifications for compliance with this guide. The examiner shall document the interview ofthe if*'ll). Performance candidate and the review of the candidate's capabilities, education, experience, vision records, training records, and ^ it 10.1 Personnel assigned the responsibility and authority % perform functions covered by this guide shall have, as a Jinimum, the appropriate level of capability given in ;-'J|ction 6. When a single inspection requires implementation a team or group, personnel not meeting the requirements this Guide may be used in data-taking assignments or in t or equipment operation provided they are supervised overseen by a qualified individual participating in the iispection. *|p.2 A certified coatings inspector shall submit annually a rnary of coatings related inspection/testing activities applicable examination records. Certifications are docu mented on a Record of Certification (Fig. 4 or equivalent form). 11.2 Coatings inspectors shall be recertified as required by 11.1 after evaluation of their work record. Individual work records shall show evidence of continuing satisfactory perfor mance. 11.3 Level I and Level II coatings inspectors are certified or recertified by a certified Level III coatings inspector. Level III coatings inspectors are certified or recertified by the responsible organization's management or by a certified Level III coatings inspector. brmed between certification anniversary dates in order to 11.4 Certification by a given employer shall be considered attain the validity of the certification. This summary for a revoked when employment is terminated. Jvel I or Level II coatings inspector shall be reviewed by a i lifted Level III coatings inspector or his designee, signed jfigiid placed in the coatings inspector's certification file. The nmary review for a Level III coatings inspector shall be fiPucted by, another certified Level III coatings inspector or responsible organization's management, signed and Ifeed in the inspector's certification file. 12. Records 12.1 A personnel qualification records file shall be estab lished and maintained by the employer. Collection, storage, and control of records required by this guide shall be in accordance with the requirements of the responsible organi zation and appropriate specifications. p),3 Any certified coatings inspector not performing coat- 13. Keywords iiiejt ,irg-> related inspection/testing work between certification 13.1 certified coatings inspector; coatings inspection; i iversary dates shall be recertified in accordance with coatings inspector; inspector certification; Level II Coatings 112, after it is reconfirmed that the inspector's capabilities Inspector; Level III Coatings Inspector; nuclear coatings ffijtet the requirements of this guide. inspector; qualified coatings inspector The American Society tor Testing and Materials takes no position respecting the vaiidity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determinatiotv-of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the respons/Jbfe technical committee and must be reviewed every five years and if not revised, either reapprovedor withdrawn..Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feei that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 783 mm DU PO50297965 Designation: D 4538 - 90a Standard Terminology Relating to Protective Coating and Lining Work for Power Generation Facilities1 This standard is issued under the fixed designation D 4538; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. alligatoring--in protective coatings, surface cracking of coating film having an appearance similar to alligator hide. certification--in protective, coatings, the written documen tation of the qualification of personnel or material. checking--in protective coatings, the formation of slight breaks in a coating film that do not penetrate to the underlying surface. coating applicator--in protective coatings, an organization or individual responsible for applying a protective or decora tive coating. coating system--in protective coatings, a protective film consisting of one or more coats, applied in a predeter mined order by prescribed methods. coating work--in protective coatings, ait all-inclusive term to define all operations required to accomplish a complete coating job; construed to include materials, equipment, labor, preparation of surfaces, control of ambient condi tions, application of coating systems, and inspection. cobwebbing--in protective coatings, the formation of fine filaments (cobwebs) or partly dried coating, during spray application. cracking--in protective coatings, the formation ofbreaks in a coating film that extend through to the underlying surface. cratering--in protective coatings, the formation of round depressions in a coating film that do not expose the previous coat or the substrate. crawling--in protective coatings, a defect in which a wet coating film recedes from a small area to form an uneven surface shortly after application. crazing--in protective coatings, the formation of a criss-cross pattern of minute cracks on the surface of a coating film. deiamination--in protective coatings, a separation of one coat from another coat within a coating system; or from the substrate. ' These definitions are under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and are the direct responsibility of Subcommittee D 33.92 on Definitions. Current edition approved Nov. 30, 1990. Pubtishsd January 1991. Originally published as D 4538 - 86a. Lust previous edition D 4538 - 90. deviation--in protective coatings, a departure of a character istic from established procedures or from specified require ments, drips--in protective coatings, the small drops of coating that collect on the edge of the coated work, dry spray--in protective coatings, a rough, powdery, non coherent film produced when an atomized coating pj] tially dries before reaching the surface, flaking--in protective coatings, the detachment of small pieces of the coating film. foreign matter--in protective coatings, insoluble fon particles such as sand, lint, dust, and dirt that get mix with the coating material before, during, or after applica tion; causing the formation of raised specks in the drift film, hairline crack--in protective coatings, a very fine crackl 1 (having a hairlike appearance) that is visible on the surface"^ of a dried coating film. heavy-centered spray pattern--in protective coatings, uneven spray pattern having more coating in the center, and less at the edges. intercoat contamination--in protective coatings, the presence*! of foreign matter between successive coats, mudcracking--in protective coatings, a particular pattern eft ' cracking in a coating with the appearance of a dried mud'a puddle (see cracking and checking), orange peel---in protective coatings, the dimpled appearance , of a dried coating film resembling the surface of an orange, pinhole--in protective coatings, minute holes through a coat, or coats that expose an underlying coat or the substrate, pinholes--small pore-like Haws in a coating that extciw entirely through the applied film and have the gen. . appearance of pin pricks when viewed by reflected 1 (see Definitions D 162). qualification--in protective coatings: The characteristics or,7. abilities gained through training or experience, or both,' that enable an individual to perform a required function. wrinkling--in protective coatings, the formation of a surface1"! appearance in a coating film resembling the skin of a prune. 2 Definitions D 16. of Terms Relating 10 Paint, Varnish, Lacquer, and Related Products (Committee D - 1 on Paint and Related Coatings and Materials). This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Ycur comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 784 DUP0502 97966 Designation: D 4540 - 91 Standard Guide for Testing interior Latex Semigloss and Gloss Paints1 This standard is issued under the fixed designation D 4540; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. ,g that small oreign mixed >plicadried ^rl. Scope 1.1 This guide covers the selection and use of procedures 'iHor testing latex semigloss or gloss paints intended for use on terior walls or trim. The test methods included are listed in ables 1 and 2. 1.2 The latex semigloss and gloss paints covered by this tide are intended for application by brushing, rolling, laying, or other means, on plaster, masonry surfaces, bod, wallboard, previously painted surfaces and other terior architectural surfaces. 1.3 This standard does not purport to address all of the ifety problems, if any, associated with its use. It is the |ponsibility ofthe user of this standard to establish appro bate safety and health practices and determine the applica bility of regulatory limitations prior to use. orach urfacc >s, 'an :enter, ssenee em o! 1 mud tics or both, ction. .urfara < of a Related s)- . Referenced Documents |2;.l ASTM Standards: ID 16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 jjp 185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints3 |D344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts3 lib 522 Test Methods for Mandrel Bend Test of Attached Organic Coatings3 j|p 523 Test Method for Specular Gloss3 |P 562 Test Method for Consistency of Paints Using the 1 Stormer Viscometer3 |b 823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D 869 Test Method for Evaluating Degree of Settling of Paint3 pD1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems3 |b 1475 Test Method for Density of Paint, Varnish, Lacquer, and. Related Products3 Ip 1640 Test Methods for Drying, Curing, or Film Forma- ft tion of Organic Coatings at Room Temperature3 D1729 Practice for Visual Evaluation of Color Differ ences of Opaque Materials3 | This guide is under the jurisdiction of ASTM Committee D-l on Paint and ated Coatings and Materials and is the direct responsibility of Subcommittee 1.42 on Architectural Finishes. Current edition approved Oct 15, 1991. Published December 1991. Originally ulilished as D 4540 - 85. Last previous edition D 4540 - 9Q. 'Armttai Book ofASTM Standards, Vois 06.01, 06.02, and 06.03. 'Annual Book ofASTM Standards, Vol 06.01. D 1736 Test Method for Efflorescence of Interior Wall Paints3 D1849 Test Method for Package Stability of Paint3 D2196 Test Methods for Rheological Properties of Non- Newtonian Materials by Rotational (Brookfield) Vis cometer3 D 2243 Test Method for Freeze-Thaw Resistance of Wa ter-Borne Paints3 D 2244 Test Method for Calculation of Color Differences from InstrumentaUy Measured Color Coordinates3 D2369 Test Method for Volatile Content of Coatings? D2486 Test Method for Scrub Resistance of Interior Latex Flat Wall Paints3 D2574 Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms3 D2805 Test Method for Hiding Power of Paints by Reflectometry3 D2831 Test Method for Evaluating the Ability of a Latex Paint to Resist Efflorescence from the Substrate3 D 3258 Test Method for Porosity of Paint Films3 D 3450 Test Method for Washability Properties of Inte rior Architectural Coatings3 D3793 Test Method for Low-Temperature Coalescence , of Latex Paint Films3 D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings3 D3928 Test Method for Evaluation of Gloss or Sheen Uniformity3 D 3960 Practice for betermining Volatile Organic Com pound (VOC) Content of Paints and Related Coatings3 D4062 Test Method for Leveling of Paints by DrawDown Method3 D4213 Test Method for Wet Abrasion Resistance of Interior Paints3 D4287 Test Method for High-Shear Viscosity Using the ICI Cone/Plate Viscometer3 D 4400 Test Methods for Sag Resistance ofPaints Using a Multinotch Applicator3 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode4 E 105 Practice for Probability Sampling of Materials5 2.2 U.S. Federal Test Methods Standard No. 141:6 2112 Application by Roller 2131 Application of Sprayed Films 2141 Application of Brushed Films 3011 Condition in Container 4 Annual Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vol 14.02. 6 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 191 11-5094. 785 \ t1I ? j DU PO50297967  D 4540 4061 Drying Time 4321 Brushing Properties 4541 Working Properties and Appearance of Dried Film 3. Terminology 3.1 Definitions: 3.1.1 For definitions of terms used in this guide, see Terminology D 16. 4. Conditions Affecting Latex Semigloss and Gloss Paints 4.1 Substrate Type--The substrate to be painted can affect not only the application properties and the physical properties of a latex paint, such as gloss and uniformity, but may also be a factor in determining the type of latex paint to be used; 4.2 Substrate Condition--Dirty, alkaline, or water-soluble surfaces may affect the practical requirements and perfor mance of these paints. 4.3 Application Properties--The application properties of paints are affected by temperature, humidity, and the texture and porosity of the surface to be painted. Application is also affected by the type and quality of equipment used. 5. Selection of Tests 5.1 Many conditions affect interior latex semigloss and gloss paints, so that different types of latex paints have been developed specifically to meet the requirements of these various conditions. Although the recommended test methods in Tables 1 and 2 edver most ofthe properties of such paints, all of the tests may not be required for each paint. If a paint is to Be used only in a warm cliniate for instance, then freeze-thaw tests or low temperature coalescence tests need not be considered. 5.2 The purchaser should first determine which properties a latex paint must have and then select only the test methods that will measure or evaluate those properties. After selecting the desired tests, the purchaser should determine which of these properties are the most important and establish the appropriate requirements or specifications for obtaining the desired properties. Since paint properties frequently tend to oppose each other, some properties may need to be attenu ated if others are to be accentuated. This balance of properties must be considered when selecting the tests and establishing their requirements. A normal range of values is indicated in many of the tests methods. 5.3 This guide docs not indicate relative importance ofthe various tests nor does it recommend specific values for each test, since the properties that are important to one purchaser may hot be important to. another. 6. Sampling 6.1 Prior to sampling, the condition of the container should be established since damage to it may cause evapora tion or skinning of the pigment or other undesirable effects in the coating. Determine the condition of the coating in accordance with 7.1 and 7.2. 6.2 Sample in accordance with Practice D 3925. Deter mine the weight per gallon in accordance with Test Method D 1475. Repeat this procedure until successive readings agree within 0.2 lb (90 g) or as agreed upon between purchaser and seller. Samples for testing may then be taken. TABLE 1 last ot Test Methods by Properties Test Method Liquid Paint Properties: Condition in container Coarse particles and foreign matter Density (weight per gallon) Fineness of dispersion Odor Color compatibility Package Stability: Accelerated heat-aged stability ' Freeze-thaw stability Microorganism resistance pH stability Sampling Settling Section ASTM Test Method 7.1 7.2 7.3 7.4 7,5 7.6 7.7 7.7.1 7.7.2 7.7.3 7.7.4 6 7.7.5 D 185 0 1475 D 1210 01849 D 2243 D 2574 E 70 D3925 D 869 Federal Test Method Standard No. 14t 3011 Paint Application and Film Formation: Application 'properties Application by brush Application by roller Application by spray Drying time Low-temperature coalescence of paints Producing uniform thickness of films Touch-up uniformity Rheological Properties: Leveling Low shear viscosity (consistency) High shear viscosity (ICi cone and plate viscosity) Sag resistance Rheological properties, non- Newtonian liquids 8.1 8.1.1 8.1.2 8.1.3 8.2 8.3 8.4 8.5 D 1640 D 3793 D823 D3928 9.1 D4062 9.2 D562 9.3 D4287 9.4 D4400 9.5 D 2196 4541 2141 2112 2131 ! Appearance of Dry Paint Film: Color difference by visual evaluation Color difference using instrumental measurements Hiding power 10.1 10.2 10.3 Specular gloss Properties of Dry Paint Film: Block Resistance >.. Efflorescence of paint film Efflorescence from substrate Flexibility Film porosity Print resistance . Scrubbabiiity (wet abrasion) 10.4 11.1 11.2 11.3 11.4 11.5 11.6 11.7 Stain removal (washability) Wet adhesion 11.8 11.9 D1729 D 2244 D 344, D 2805 D 523 D 1736 D 522 3258 D 4213 or D 2486 D 3450 Analysis of Paint: Chemical analysis Nonvolatile content Volatile organic compound (VOC) 12.1 12.2 12.3 D 2369 D 3960 6.3 Specify the identification codes. A 1 U.S. gallon (orj 4-L) sample is usually sufficient for the recommended testa, but for guidance in selecting a sampling plan, consult. Practice E 105. 7. Liquid Paint Properties 7.1 Condition in the Container-Thickening, settling, a separation are undesirable and objectionable if the pafflii cannot be reconditioned with a reasonable amount off stirring. The referenced method covers procedures for deter mining changes in properties of paints after storage. Deter-g 786 DUP050297968 # D 4540 TABLE 2 Alphabetical List of Test Methods ral \ od erd * Mf 41 Test Method Section ASTM Test Method Federal Test Method Standard No. 141 ..g&ce'aratod heat-aged stability 7.1.1 Implication properties 8.1 4541 '*s^5licalion by brush replication by roller 8.1.1 8.1.2 2141 2112 pkj - walc^i by spray 8.1.3 wfock resistance Itong properties 11.1 8.1.1 l^ghemcal analysis 12.1 JjgjBgrsa particles and foreign matter 7.2 jr compatibility 7.6 jjffiafor difference using instrumental 10.2 D 2244 ' 1rements ^sgoior difference by visual evaluation ibndition In container Ipreistency (viscosity) Ss/isily (weight per gallon) frying time ^ florescence of pairit film 1ffo,'escence from substrate (m Porosity n i^eness of dispersion exibility haw stability I mtti'ing power l ar,viscosity piling , temperature coalescence of paints ^roorganism resistance jlrtvoiatne content (see volatile 10.1 ; 7.1 9.2 7.3 8.2 11.2 11.3 11.5 7.4 11.4 7.7.1 10.3 9.3 9.1 8.3 7.7.3 12.2 D 1729 D 562 D 1475 D 1640 D 1736 D 2831 D 3258 D1210 D522 D2243 D 344, D 2805 0 4287 D 4062 O 3793 D 2574 <Tqoritent) 9cr i stability 7.5 7.7 7.7.4 D 1849 E 70 I resistant |uclng uniform sickness'films "logical properties of non- 11.6 8.4 9.5 D 823 D 2196 ^Nayi/tonian liquids ] resistance npllng pubbability (wet abrasion, scrub ''distance) 9.4 6 10.7 7.7.6 D 4400 D 3925 D 2486, D4213 0 869 Specular glops n removal (washability) uch-up uniformity ^o'atiie content tfafatile organic compound (VOC) " `et adhesion 10.4 11.8 8.5 12.2 12.3 11.9 D 523 D 3450 03928 D2369 D 3960 Ine the condition in the container in accordance with ethod 3011 of Federal Test Method Standard No. 141. Be also 7.7 on Package Stability:) 117.2 Coarse Particles and Foreign Matter: |7:2.1 Paints must be free of coarse particles to form aifcrm films of good appearance, a typical maximum being jjpeight % of total paint, The specified test with a 325-mesh S-pm) screen and water as the wash liquid gives the percent ll'ihese particles in a latex paint. Determine coarse particles |fd foreign matter in accordance with Test Methods D 185. 17.2.2 Another test method used in industry to determine giether coarse particles are present in a dry film is to scrape : surface of the film with a spatula or metal edge of a ruler, ay particles larger than 325 mesh (45 pm) can be clearly geen after the surface has been scraped. . M 7.3 Density (Weight per Gallon)--The density as mea sured by weight per gallon (kilograms per litre) is used to assure product uniformity from batch to batch. It does not necessarily measure the quality of a paint. In the referenced method, the density is expressed as the weight in pounds per U.S. gal (or kg/L) of the paint at a specified temperature. Most interior semigloss and gloss paints have densities of about 10 to 12 lb/gal (1.2 to 1.4 kg/L). Determine density in accordance with Test Method D 1475. 7.4 Fineness ofDispersion: 7.4.1 The more finely a pigment is dispersed, the more efficiently it is being used. One method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the material down a calibrated tapered groove varying in depth from 4 to 0 mils (100 to 0 pm). The Hegman scale is one commonly accepted measurement method. The point at which the continuous groupings of particles or agglomerates, or both, protrude through the surface of the liquid is taken as the fineness reading. Lower readings in mils or micrometres or higher readings in Hegman units indicate better fineness dispersion. Measure fineness of dispersion in accordance with Test Method D 1210. 7.4.2 The referenced method was designed primarily for coatings with good fineness of dispersion such as enamels. Most interior semigloss and gloss latex paints have a fineness of about 7.5 to 5 Hegman (6 to 40 pm). 7.5 Odor--One of the advantages of latex paints is that they do not have odors characteristic of solvent-reducible coatings. However, other ingredients, such as ammonia, may be used that might also be objectionable in confined spaces. Thus, interior latex paints should be tested for odor accept ability. Determine whether the paint has an unpleasant or irritating odor during application or drying. 7.6 Color Compatibility--A test method to determine how well colorants can be dispersed in paints so that the paint will have uniformity of color when applied is in preparation and will be included in the guide when adopted by AS TM. > 7.7 Package Stability--Since paints cannot normally be used immediately after manufacture they must remain stable in the can for some time, At normal temperatures, most latex paints can be stored for over a year with little change in properties. Although indications of long term package sta bility can usually be obtained in several days or weeks at an elevated temperature, such as 140F (60C) or 122F (50C), occasionally the results of the accelerated test do not agree with those at prolonged normal storage conditions. The referenced method predicts the change in consistency and certain other properties in packaged latex paint when stored at temperatures above freezing. Determine package stability in accordance with Test Method D 1849. 7.7.1 Heat Stability--Heating is used to accelerate changes in viscosity with time and to predict their affect on other properties. An excessive increase or decrease in vis cosity after heat-aging is unacceptable. There is a general correlation between short-term high temperature oven sta bility and long-term shelf storage at ambient temperature. This test is meant to predict which paints will not be stable when stored by customers or consumers under elevated temperature for a short period of time or at room tempera ture for a longer period of time. After heat-aging, such 787 DU PO 502 97969 D 4540 properties as viscosity, flow, gloss, pH drift, foam resistance, color uniformity, and wet adhesion are usually rechecked versus room temperature-aged controls. 7.7.2 Freeze-Thaw Stability--Water-reducible paints may be subjected to freezing conditions during shipping and storage. Suitably stabilized paints will resist several cycles of freezing and thawing without showing deleterious changes such as coagulation, graininess, or excessive viscosity in crease. Many latex paints will increase in viscosity but can still be considered satisfactory if other properties that may be affected by a higher viscosity) such as leveling and brushability, are satisfactory. Determine freeze-thaw stability in accordance with Test Method D 2243. 7.7.3 Microorganism Resistance--Bacteria in a latex paint can cause gassing, putrefactive or fermentative odors, and loss of viscosity. Determine if the paint contains living bacteria or if it is resistant to attack by bacteria in accordance with Test Method D 2574. : 7.7.4 pH--Latex paints with low (acidic) pH can corrode metai containers. pH may. vary from about 5 to 10 de pending upon the type of latex used and general formulation. pH does not determine the quality of a latex paint and should only be used to assure product uniformity. However, a change in pH during storage may indicate poor stability and unacceptable change in the properties of a paint. Determine pH in accordance with Test Method E 70. 7.7.5 Settling--Latex paints are generally resistant to hard settling, but do at times show separation and soft settling. The referenced method covers the. degree of pigment suspen sion and ease of remixing a shelf-aged sample of paint to a homogeneous condition suitable for the intended use. Deter mine settling in accordance with Method D 869. 8, Paint Application and Film Formation %A Application. Properties--Determine the ease1 with tehich a paint can be applied to various wall surfaces with brush, roller, or Spray equipment, in accordance with Method 4541 of Federal Test Method Standard No: 141. Application properties are generally compared to a standard, or described by requirements in a product specification. 8.1.1 Brush Application--Brushed films should be smooth and free of seeds and on verticaf surfaces should show no sagging, color streaking, or excessive brush marks. The specified method covers the determination of the brushing properties of coatings. The test is subjective al though those experienced in the art Can' produce quite consistent results, particularly in the evaluation of "drag" properties. Determine brushing properties in accordance with Method 4321 of Federal Test Method Standard No. 141. 8.1.2 Roller Application--Walls are frequently painted with rollers that produce slight stipple effects. Determine the ease with which a paint can be roller applied in accordance with Method 2112 of Federal Test Method Standard No. 141. Since roller foam and roller spatter are often serious problems when latex paints are roller applied, these proper ties can also be determined in the test method for roller application; The amount of foam produced, the time that it takes for the bubbles to break, and the number ofcraters that remain after the bubbles have broken can be determined by visual examination of the test panel. Roller spatter can be determined by placing a strip of paper or a panel at the bottom of the test panel to catch the paint spatters from the roller. The degree to which a paint will spatter when roller applied can be determined by the density ofthe paint spatter..: 8.1.3 Spray Application--Interior coatings are sometimes?: applied by spray. Both air and airless spray are used 0n commerical work. Determine the spray application propen : ties in accordance with Method 2131 of Federal Test Methdifl Standard No. 141. The method can be modified to include application by airless spray equipment. 2| 8.2 Drying Properties--The drying time of an interior latex paint is important in determining when a freshly painted room can be put back to use. Under average conditions most semigloss and gloss latex paints are dry fjf touch in 1 to 2 h when the water has evaporated from the film. Because of the glycols usually present in these paints it" is prudent to recoat after at least an 18-h dry. I properties may take a few days to develop'for stime i i. paints while cithers may require a few weeks depend] nr the composition. Determine the drying time in accordaijh|| with Test Methods D 1640. 8.3 Low-Temperature Coalescence of Paints--T1 enced test method determines how well the latex partieiSS a paint Mil fuse together or coalesce, to form a contiiM'.ii, ] film at low temperatures. Determine low-temperatun cence in accordance with Test Method D 3793. 8.4 Producing Films of Uniform Thickness--The lowing method covers the preparation of various fi' n; o r uniform thickness essential in conducting tests. Prepare flints! in accordance with Test Methods D 823. 8.5 Touch-Up Uniformity--After paint has dried, where less material was applied sometimes become : able. If the paint has suitable touch-up properties, ad paint can be applied to these areas only, instead of reftuf ishing the complete wall. The color, gloss, and leveling of t touched-up areas and the previously painted area should.1 uniform. Differences in these properties are often caused:! short wet edge time, poor leveling on recoat and orientation or floatation during and after application, mine touch-up properties in accordance with Test Me D 3928. 9. Rheological Properties 9.1 Leveling--Leveling is an important factor when i form surfaces are to be produced as it affects hiding ] and appearance. Brush marks, and imperfections are : more conspicuous in semigloss and gloss paints than they?! in flat paints. The referenced method covers the characteristics of liquid coatings. Evaluate leveling in accet-^ dance with Test Method D 4062. 9.2 Low Shear Viscosity (Consistency)--Paints of a j type should fall within a stated consistency ran satisfactory reproduction of a specific formula. While consiS-.: tency is an important property, it does not determine the;,; quality of a paint and should be used mainly to enspfl product uniformity. In the referenced method, cbnsistencyj;|lS defined as the load in grams to produce a specified rate of' shear. Although the consistency of most latex wall paint \ about 150 to'300 g, a much wider range is possible because the wide variations in rheological properties of these paints? Two paints of the same consistency may have quite diffei|fw 788 DUP0502 97970 D 4540 t the om the 1 Jo icr spatter etimes 9 it on proper. 1huc nclude nterior ftovhh verage dry to 'in the Hits it hm, t: lat., H. on dance" e fd-i ms of films 'areas IlllL. ttonal refm- * ed by rtlC )ete urn-^ mm nilflijl y are* ' elmg? ccor-' |bgical properties since this is only a measure of their ifshear viscosity. Optimized application properties are illy used to determine the optimum consistency. Meahe consistency in accordance with Test Method D 562. |3 High Shear Viscosity (IC1 Cone and Plate Viscos-The shear rate for this measurement (10 000 reciprocal ttds) is similar to that occurring during brush applicai, and the viscosity measured at this shear rate therefore is 1 to brush drag, which is in turn related to spreading l^jand film build. Measure the high shear viscosity in ance with Test Method D 4287. ! Sag Resistance--This is an important property particfor semigloss and gloss latex paints because sagging i in unsightly film appearance. Measure the sag fesis- i in accordance with Test Methods D 4400. Rheological Properties, Non-Newtonian Liquids-- ^logical properties are related to application and leveling ties of the liquid paint. The referenced methods cover Idetermination of rheological properties, and are particu- suited for use with paints that display thixotropic icteristics. They 'actually measure viscosity under dift shear rates. Determine rheological properties in accorIK with Test Methods D 2196 or D 4287, or both! |ppearance of Dry Film ` (jl Color Differences by Visual Evaluation--Visual rison of color is fast and often acceptable although erica! values are not obtained. The referenced method ; the spectral, photometric, and geometric characterisf light source, illuminating and viewing conditions, size imens, and general procedures to be used in the visual ation of color differences of opaque materials. Deter ge color differences in accordance with Practice D 1729. p.2 Color Differences Using Instrumental Measure rs--The differences in color between a product and its trd can be measured by instrument. Generally, the nee is agreed upon by the purchaser and the seller and also be required if a product specification is involved. iBr instruments provide numerical values that can be Spared to subsequent measurements. The referenced 1 covers the instrumental determination of small color iflcrences observable in daylight illumination between tameric, opaque surfaces such as coated specimens. If j$unerism is suspected, visual evaluation (see 10.1) should lised to verify the results. Calculate in accordance with ! Method D 2244 the color differences that have been red instrumentally. |10.3 Hiding Power (Dry Opacity)--Hiding power is the ure of the ability of a paint to hide the substrate. It is, ever, dependent upon uniform film thickness that is ptienced by flow and leveling. Test Method D 344 is a test in which paint is applied with a brush, film tkness is approximately measured, opacity is evaluated bally compared to a standard paint, and results are ed by flow and leveling application properties of the it. Test Method D 2805 is considered to be a more tecise and accurate test that does not need a material paint < iard. Paint is applied with an applicator bar to minimize effects of flow and leveling, film thickness is rigorously \jsured, and opacity is instrumentally evaluated. Deter mine hiding power in accordance with Test Methods D 344 or D 2805. 10.4 Specular Gloss--The method given, using the 20 geometry for high gloss paints and ,60 geometry for semigloss paints, is useful in characterizing the direct appear ance of gloss and semigloss paints. According to the Paint/ Coatings Dictionary,7 the semigloss range is usually 35 to 70 using the 60 geometry. Full gloss is usually above 70 using the 60 geometry. Although paints with good uniformity of appearance are often paints of lower gloss and paints with good cleanability are often' ones with higher gloss, this is not always the case, and the gloss of a paint should not be used as a measure of other paint properties. Determine the gloss at 20 and 60, as appropriate, gloss in accordance with Test Method D 523. 11. Properties of Dry Film 11.1 Block Resistance--This is an important property of an interior semigloss or gloss since it is the resistance of the painted surfaces to stick together when stacked or placed in contact \tfith each other. An interior paint often comes in contact with itself especially in the cases of doors, windows and drawers and sometimes sticks to itself: (blocks) de pending on the hardness of the coating, the pressure, temperature, humidity, and duration of time the surfaces are in contact. 11.2 Efflorescence of the Paint Film--The referenced method measures efflorescence that comes from the paint itself,- not from the substrate. Few interior latex paints effloresce due to improvements in latex and latex paint formulations. Salt formation is produced by specific condi tions of temperature and humidity if a paint contains sufficient solid water-soluble material to cause a noticeable deposit on the film. Determine efflorescence resistance in accordance with Test Method D 1736. 11.3 Efflorescence from Substrate--Cementitious sub stances may contain sufficient solid water-soluble materials to cause a surface deposft through leaching and evapora tion. 11.4 Flexibility--Elongation is a measure of the flexibility of a paint film. Most interior latex paints can be bent over a `/8-in. (3.2-mm) mandrel without affecting the film. Deter mine elongation in accordance with Test Methods D 522. 11.5 Film Porosity--The more porous a paint is, the worse will be its cleanability and enamel holdout. Determine film porosity in accordance with Test Method D 3258. 11.6 Print Resistance--The ability of a coating to resist printing is important because its appearance is adversely affected if the surface texture is modified by contact with another surface particularly one with a pattern. Interior gloss and semigloss systems on window sills and other horizontal surfaces often have flower pots placed on them that may tend to leave a permanent impression from the pressure. This tendency for a paint film to "print" is often a function of tfie hardness of the coating, the pressure, temperature, humidity, and duration of time that the painted surface is in contact with the object. 7 Available from Federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA i 9422. 789 I DUP050297971 ID 4540 11.7 Scrubbability--The ability of an interior finish to resist scrubbing is an important property. The referenced method provides a measure ofthe wet abrasion resistance of a film. However, wet abrasion resistance is not necessarily a measure of how well soils or stains can be removed since some paints have good scrubbability but poor stain cleanability because they are porous. Determine the scrubbability in accordance with Test Method D4213 or D 2486. A control paint should always be tested at the same time because of the variability of the method. 11.8 Slain Removal (Cleanability)--The ability to remove marks satisfactorily without damaging the film is an import tant property of interior finishes. Determine stain removal in accordance with Test Method D 3450, 11.9 Wet Adhesion--It is essential that an interior finish adhere tightly to a given substrate or primer under the wet conditions of washing or scrubbing. 12. Analysis of Paint 12.1 Chemical Analysis--If a specification requires cer tain raw materials or certain components in a given amount, then chemical analysis is required to determine whether the specified materials are present and in what amounts. Anal ysis does not necessarily establish paint quality that can also be greatly affected by manufacturing techniques. Most ASTM analytical methods apply to solvent-based coatings. However, some of them can be adapted for analysis of latex paints. 12.2 Volatile Content--The percent of volatile matter is a measure of the amount of a liquid coating lost as it dnes t This quantity is not necessarily indicative of the quality ' f coating. It is useful, however, for determining the similarity] of two batches. The referenced method-covers the determi nation of the volatile content by weight of solvent- andl water-reducible coatings. The quantity determined sub-' traded from 100 % gives the nonvolatile content. Determine S volatile content in accordance with Test Method D 2369. 12.3 Volatile Organic Compound (VOC) Content-- eral local jurisdictions in California have adopted air pollu.1 tion controls that severely limit the amount of solvent (Volatile Organic Compound (VOC) content) permitted m architectural coatings, including interior latex gloss and. semigloss paints. Since these paints may contain solvents l such as coalescents and cosolvent wet edge aids, it is essential that these products not exceed the established VOC limits.,. Determine VOC content in accordance with Practice I D 3960. 13. Field Testing 13.1 Although many of the recommended test methods* attempt to simulate conditions under which latex seimgi.i and gloss wall paints are applied, it is not possible to Is accurately simulate all possible conditions. Testing l;.u:. semigloss and gloss wall paints under field conditions jg] recommended for the final evaluation of suitability. 14. Keywords 14.1 architectural coatings; gloss paints; interior paints, ( latex paints; semigloss paints The American Society lor Testing end Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk bl Infringement ot such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either forrevision ot this standard or tor additional standards and should be addressed (a ASTM Headquarters. Your comments will receive caretul consideration at a meeting ot the responsible technical committee, which you may attend. If you fee) that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 790 DUP0502 97972 Designation: D 4541 - 85 (Reapproved 1989) Standard Test Method for Pull-Off Strength f Coatings Using Portable Adhesion Testers1 This standard is issued under the fixed designation D 4541; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1 NRS' --Editorial changes were made throughout in April 1989. I 'icope 1.1 This test method covers a procedure and apparatus for ilLdting the pull-off strength (commonly referred to as adhesion") of a coating by determining either the greatest endicular force (in tension) that a surface area can bear fore a plug of material is detached, or whether the surface nuns intact at a prescribed force (pass/fail). Failure will ur along the weakest plane within the system comprised i the test fixture, adhesive coating system, and substrate and be exposed by the fracture surface. This test method simizes tensile stress as compared to the shear stress plied by other methods such as scratch or knife adhesion il TG suits may not be comparable. 1.2 This test method uses a class of apparatus known'as nll-off adhesion testers.2 They are portable and capable of Implying a concentric load and counter load to a single rface so that coatings can be tested even though only one |fde is accessible. Measurements are limited by the strength adhesion bonds between the loading fixture and the ecimen surface or the cohesive strength of the substrate. 1.3 This test can be destructive and spot repairs may be ri'.cssaiy. ("T.4 This standard may involve hazardous materials, operOK-. and equipment. This standard does hot purport to i: iar s > all ofthe safety problems associated with its use. It is 11' u sponsibility of the user of this standard to establish nwopriate safety and health practices and determine the 'ppheability of regulatory limitations prior io use. For pecific hazard statements, see Notes 2 and 3. Kelerenced Documents E 2,1 ASTM Standards: D2651 Practice for Preparation of Metal Surfaces for Vlhesive Bonding3 D 1^33 Practice for Preparation of Aluminum Surfaces for Structural Adhesives Bonding (Phosphoric Acid Anodizing)3 2.2 ANSI Standard: 1 Tus *est method is under ihe jurisdiction of ASTM Committee D-t on Paint 5c Related Coatings and Materials and is the direct responsibility of SubcomTKlec D0I.4G on Industrial Protective Coating. Current edition approved Nov. 29. 1985. Published January 1986. rm adhesion tester may be somewhat of a misnomer, but its adoption by two manufacturers and at least two patents indicates continued usage. / Book ofASTM Standards, Vol 15.06. N512 Protective Coatings (Paints) for the Nuclear Industry4 2.3 ISO Standard: 4624 Paints and Varnish--Pull-Off Test for Adhesion4 3. Summary of Test Method 3.1 The general pull-off test is performed by securing a loading fixture (dolly) normal (perpendicular) to the surface of the coating with an adhesive. After the adhesive is cured, a testing apparatus is attached to the loading fixture and aligned to apply tension normal (perpendicular) to the test surface. The force applied to the loading fixture is then gradually increased and monitored until either a plug of coating material is detached, or a specified value is reached. When a plug of material is detached, the exposed surface represents the plane of limiting strength within the system. The nature of the failure is qualified in accordance with the percent of adhesive and cohesive failures, and' the: actual interfaces and layers involved. The pull-off strength is computed based'. on the maximum indicated load, the instrument calibration data, and the original surface area stressed (see Fig. 1). ,, . 4. Significance and Use . 4.1 The pull-off strength (commonly referred to as adhe sion) of a coating is an important performance property that has been used in specifications. This test method serves as a means for uniformly preparing and testing coated surfaces, and evaluating and reporting the results. This test method is applicable to any portable apparatus meeting the basic requirements for determining the pull-off strength of a coating. 5. Apparatus 5.1 Adhesion Tester, commercially, available, or compa rable apparatus specific examples of which are listed in Annexes A1 and A2 (see Fig. 1): 5.1.1 Loading Fixtures, having a flat surface on one end that can be adhered to the coating and a means of attach ment to the tester on the other end. 5.1.2 Detaching Assembly (adhesion tester), having a central grip for engaging the fixture. 4 Available from American National Standards Institute, 11 W. 42nd St., 13th Floor, New York, NY 10036. 791 DUP0502 97973 # D 4541 FIG. 1 Schematic of Pull-Off Adhesion Tester 5.1.3 Base, on the detaching assembly, or an annular bearing ring if needed for uniformly pressing against the coating surface around the fixture either directly, or by way ofan intermediate bearing ring. A means of aligning the base is needed so that the resultant force is normal to the surface. If shims are required when a bearing ring is employed, place them between the tester base and bearing ring rather than on the coating surface. 5.1.4 Means of moving the grip away from the base in as smooth and continuous a manner as possible so that a torsion free, co-axial (opposing pull of the grip and push of the base along the same axis) force results between them. 5.1.5 Timer, or means of limiting the rate of stress to less than 150 psi/s (1 MPa/s) so that the maximum stress is obtained in less than about 100 s. A timer would be the minimum equipment when used by the operator along with the force indicator in 5.1.6. 5.1.6 Force Indicator and Calibration Information, for determining the actual force delivered to the loading fixture. 5.2 Solvent, or other means for cleaning the loading fixture surface; Finger prints, moisture, and oxides tend to be the primary contaminants. 5.3 Fine Sandpaper, or other means of cleaning the coating that will not alter its integrity by chemical or solvent attack. If any light sanding is anticipated, choose only a very fine grade abrasive that will not introduce flaws or leave a residue. 5.4 Adhesive, for securing the fixture to the coating that does not affect the coating properties. Two component epoxies5 and acrylics6 have been found to be the mov versatile. 5.5 Magnetic or Mechanical Clamps, if needed, I p holding the fixture in place while the adhesive cures. 5.6 Cotton Swabs, or other means for removing excess adhesive and defining the adhered area. Any method for removing excess adhesive that damages the surface, such ;x scoring, must generally be avoided since induced surface flaws may cause premature failure of the coating. 5.7 Circular Hole Cutter (optional), to score through to the substrate around thedoading fixture. 6. Test Preparation 6.1 The method for selecting the coating sites to 1: prepared for testing depends upon the objectives of the test1 and agreements between the contracting parties. There are, however, a few physical restrictions imposed by the general method and apparatus. The following requirements apply t' all sites: 6.1.1 The selected test area must be a flat surface lai 1 enough to accommodate the specified number of replicate tests. The surface may have any orientation with reference r gravitational pull. Each test site must be separated by at least ~ the distance needed to accommodate the detaching appa-.; 5 Araldite Adhesive, available from Ciba-Geigy Plastics, Duxford, Cambridge, CB2 4QA, England, Scotch Weld Adhesive I838B/A, available from 3M, Adhesive Coatings amd Sealers Div., 3M Center, St. Paul, MN 55144. and Hysol Epoxy Patch Kit 907, available from Hysol Div., The Dexter Corp., Willow Pass Rd,, Pittsburg, CA 94565, have been found satisfactory for this purpose. 6 Versiloc 201 and 204 with accelerator, available from Lord Corp., Industrial Adhesive Div., 20 J 0 W. Grandview BJvd., P.O. Box 10038, Erie, PA 16514, have been found satisfactory for this purpose. 792 DUP050297974 Bus. The size of a test site ts essentially that of the secured 'ng fixture. At least three replications are usually re'd in order to statistically characterize the test area.. 6.1.2 The selected test areas must also have enough endicular and radial clearance to accommodate the ratus, be flat enough to permit alignment, and be rigid ugh to support the counter force. 6.2 Since the rigidity of the substrate affects pull-off ngth results and is not a controllable test variable in field -urements, some knowledge of the substrate thickness composition should be reported for subsequent analysis .laboratory comparisons. For example, steel substrate of than '/s-in. (3,2-mm) thickness may reduce pull-off ngth results compared to 'A in. (6.4 mm) thick panels. 6.3 Subject to the requirements of 6.1, select representas test areas and clean the surfaces in a manner that will t affect integrity of the coating or leave a residue. Surface sasion may introduce flaws and should generally be 'ed. A light abrasive should only be used if needed to hove loose or weakly adhered surface contaminants. 6.4 Clean the loading fixture surface as indicated by the aratus manufacturer. Failures at the fixture-adhesive 7-rface can often be avoided by treating the fixture surfaces ordance with an appropriate ASTM standard practice preparing, metal surfaces for, adhesive bonding. TU' 1--Practices D 2651 and D3933 are typical of well-proven i.tbods for improving adhesive bond strengths to metal surfaces. 15 Mix the adhesive 'in accordance with the adhesive lufacturer's recommendations, applying the adhesive reen the fixture and the surface to be tested using a %iod preferred by the adhesion-tester manufacturer. Carey remove the excess adhesive from around the fixture. -VE . 2: Caution--Movement, especially twisting, can cause tiny les to coalesce into large holidays that constitute stress /ntmuities during testing. i|;6 Based on the adhesive manufacturer's recommenda*hs and the anticipated environmental conditions, allow ough time for the adhesive to set up and reach the mmended cure. During the adhesive set and early cure a constant contact pressure should be maintained on -fixture. Magnetic or mechanical clamping systems work 1, but systems relying on tack, such as masking tape. Id be used with care to ensure that they do not relax time and allow air to intrude between the fixture and Test area. i|.7 Scoring around the fixture violates the fundamental |situ test criterion that an unaltered coating be tested. If 'ng around the test surface is employed, extreme care is ired to prevent micro-cracking in the coating. Such !cks may cause failures at diminished strengths. Scored pples constitute a different test, and this procedure should fclearly reported with the results. 6.8 Note the approximate temperature and relative flu idity during the time of test. lest Procedure 7.1 Select an adhesion-tester with a detaching assembly ing a force calibration spanning the range of expected lies along with its compatible loading fixture. Mid-range surements are usually the best, but before proceeding, read the manufacturer's operating instructions. 7.2 If a bearing ring or comparable device (5.1.3) is to be used, place it concentrically around the loading fixture on the coating surface. 7.3 Carefully connect the central grip of the detaching assembly to the loading fixture without bumping, bending, or otherwise prestressing the sample and connect the de taching assembly to its control mechanism, if necessary. For nonhorizontal surfaces, the detaching assembly should be manually supported so that its weight does not contribute to the force exerted in the test. 7.4 Align the device according to the manufacturer's instructions and set the force indicator to zero. NWX' 3: Caution-- Proper alignment is critical. If shims are needed for fixed alignment devices, report the manner in which used. 7.5 Increase the load to the fixture in as smooth and continuous a manner as possible, at a rate of less than 150 psi/s (1 MPa/s) so that failure occurs, or the maximum stress is reached in about 100 s or less. 7.6 Record the force attained at failure or the maximum force applied. 7.7 If a plug of material is detached, label and store the fixture for qualification of the failed surface in accordance with the procedure in 8.3. 7.8 Report any departures from the procedure such as possible misalignment, hesitations in the force application, etc. 8. Calculation and Interpretation of Results 8.1 Use the instrument calibration factors to convert the indicated force for each test into the actual force applied in units of pounds-force. (1 N = 0.1 kgf). 8.2 Compute the relative stress applied to each coating sample as follows: X = AF/d2r where: X = greatest mean pull-off-stress applied during a pass/fail test, or the pull-off strength achieved at failure. Both have .units of psi (MPa = 1 N/mm2). F = highest force applied to the test surface as determined in procedure in 8.1, and d = equivalent diameter of the original surface area stressed having units of inches (or millimetres). This is usually equal to the diameter of the loading fixture. 8.3 For all tests to failure, estimate the percent ofadhesive and cohesive failures in accordance to their respective areas and location within the test system comprised ofcoating and adhesive layers. A convenient scheme that describes the total test system is outlined in procedures in 8.3.1 through 8.3.3. (See ISO 4624.) 8.3.1 Describe the specimen as substrate A, upon which successive coating layers B, C, D, etc., have been applied, including the adhesive, Y, that secures the fixture, Z, to the top coat. 8.3.2 Designate cohesive failures by the layers within which they occur as B, C, etc., and the percent of each. 8.3.3 Designate adhesive failures by the interfaces at which they occur as A/B, B/C, C/D, etc., and the percent of each. 8.4 Erratic errors should be dropped. Unpredictable errors 793 DUP050297975 D 4541 may result if alignment of the apparatus is not normal to the surface, from poor definition of the area stressed due to improper preparation of the adhesive, poorly defined glue lines and boundaries, holidays in the adhesive caused by voids, inclusions, improperly prepared surfaces, or sliding or twisting the fixture during the initial cure. Scratched or scored samples may contain stress concentrations leading to premature fractures. These should be retested at adjacent areas. 8.5 Further information relative to the interpretation of the test results is given in Appendix Al. 9. Report 9.1 Report the following information: 9.1.1 Brief description of the general nature of the test, such as, field or laboratory testing of the general type of coating as applied to a given substrate, etc. 9.1.2 Temperature and relative humidity and any other pertinent environmental conditions during the test period. 9.1.3 Apparatus used, fixed or self-aligning, which in cludes: apparatus manufacturer and model numbers, loading fixture type and dimensions, and bearing ring type and dimensions. 9.1.4 Description of the test system, if possible, by the indexing scheme outlined in 8.3 including: product identity and generic type for each coat and any other information supplied, the substrate identity (thickness, type, orientation, etc.), and the adhesive used. 9.1.5 Test results. 9.1.5.1 Date, test location, testing agent. 9.1.5.2 For pass/fail tests, stress applied along with thel result, for example, pass or fail and note the plane of am,1 failure (see ANSI N512). y' 9.1.5.3 For tests to failure, all values computed in (j.J jalong with the nature and location of the failures as specified in 8.3, or, if only the average strength is required, report it along with the statistics. 9.1.5.4 If corrections of the results have been made, or if certain values have been omitted such as the lowest cit '. highest values or others, reasons for the adjustments and criteria used. 9.1.5.5 For any test where scoring was employed, indicate it by placing a footnote superscript beside each data point affected and a footnote to that effect at the bottom of each! page on which such data appears. Note any other deviations from the procedure. 10. Precision and Bias 10. i The precision and bias is primarily dependent upon the accuracy of the force measurement, the alignment of the device, and the care exercised in preparation and testing. " 10.2 Since no standard for pull-off strength ofcoatings ti||| been developed prior to this test method, precision and bi| statements will be developed in round-robin testing. 11. Keywords 11.1 adhesion; adhesive strength; bond strength; coatings;, cohesion; cohesive strength; paints; pull-off strength 794 DUPO 502 97976 vith the : of any 1 in 8.2 pecified 'eport it ie, or if west or nts and ndicate a point of each nations t upoti t of the ing ngs has rd bias.: atingsjl ANNEXES (Mandatory Information) |.l. FIXED-ALIGNMENT ADHESION TESTERS--ELCOMETER MODEL 106 ADHESION TESTER (Fig. Al.l)7 A 1.1 Apparatus: A 1.1.1 This is a fixed-alignment portable tester. A 1.1.2 The tester is comprised of detachable aluminum lading fixtures having a flat conic base that is 0.8 in. in mneter on one end for securing to the coating, and a rcular T-bolt head on the other end, a central grip for ging the loading fixture that is forced away from a tripod by the interaction of a handwheel (or nut), and a xial bolt connected through a series of belleville :hers,or springs in later models, that acts as both a torsion f and a spring that displaces a dragging indicator with ect to a scale. A1.1.2 The force is indicated by measuring the maximum ing displacement when loaded. Care should be taken to that substrate bending does not influence its final ition or the actual force delivered by the spring arrange- ent. i , Al. 1.4 The devices are available in four ranges: from 0 to 0 to 1000. 0 to 2000, and 0 to 4000 psi (35, 70, 140 and 10 kgf/cm2). A 1.2 Procedure: A 1.2.1 Center the bearing ring on the coating surface ncentric with the loading fixture. Turn the hand wheel or nut of the tester counter-clockwise, lowering the grip so that slips under the head of the loading fixture. A 1.2.2 Align or shim the three instrument swivel pads of tripod base so that the instrument will pull perpendicu- Jy to the surface at the bearing ring. '1.2.3 Take up the slack between the various members id slide the dragging (force) indicator located on the tester zero. . V1.2.4 Firmly hold the instrument with one hind. Do not nw the base to move or slide during the test. With the er hand, turn the handwheel clockwise using as smooth constant a motion as possible. Do not jerk or exceed a os rate of 150 psi/s (1 MPa/s) which is attained by owing in excess of 7 s/1000 psi stress. If the 2pOO or., 4000 models are used, the handwheel is replaced with a nut [uiring a wrench for tightening. The wrench must be used V; 7 Manufactured by Elcomcter Instruments, Ltd,, Edge Lane, Droylston, Manchester 356UB, England. ' FIG. All Elcometer Model 106 Adhesion Tester itfa plane parallel to the substrate so that the loading fixture will not be removed by a shearing force or misalignment thus negating the results. The maximum stress must be reached within about 100 s. A 1.2.5 The pulling force applied to the loading fixture is increased to a maximum or until the system fails at its weakest locus. Upon failure, the scale will rise slightly, while the dragging indicator retains the apparent load. The appa ratus scale indicates an approximate stress directly in pounds per square inch, but may beifiompared to a calibration curve. Al .2/6 Record the highest Value attained by reading along the bottom of the dragging indicator. 795 DUP050297977 D 4541 A2. SELF-ALIGNING ADHESION TESTERS--SEMICRO PNEUMATIC ADHESION TESTER (Fig, A2.1)8 A2.I Apparatus: A2.1.1 This is a self-aligning tester, although a non self-aligning pneumatic apparatus is in use in Europe.9 It is portable and has a common pressure source and measuring system that controls a choice of different range detaching assemblies. A2.1.2 The apparatus is comprised of: (7) detachable loading fixtures having a flat cylindrical base that is 0.5 in. (13 mm) in diameter on one end, for securing the coating, and % UNC threads on the other end; (2) a central grip for engaging the loading fixture through an annular base that is forced away from the grip by the interaction of a self-aligning seal; and (i) a pressurized gas that enters the device through a flexible hose connected to a pressurization rate controller and a pressure gage (or electronic sensor). A2.1.3 The force is indicated by the maximum gas pressure when loaded, which is not displacement dependent, and can be directly calibrated. A2.1.4 The detaching assemblies are available in four standard ranges in multiples of two from 0 to 500 psi (3.5 8 Manufactured by SEMiero Carp., 15817 Crabbs Branch Way, Rockville, MD 20855. 9 Saberg Apparatus, available from Scandinavian Paint and Priming Inc., Research Institute, Copenhagen, Denmark. MPa) to 0 to 4000 psi (28 MPa). Special ranges to 10 000 pS; (70 MPa) are available. A2.1.5 The standard System 2000 is a fully automated electronic monitoring and control system of briefcase size that can be used with any detaching assembly. Special manually controlled pneumatic devices can be ordered. A2.2 Procedure: A2.2.1 Position the annular ring on the coating concentric with the fixture, and loosely engage the fixture via the central threaded grip. Leave at least '/si-in. (0.8-mm) clearance between the detaching assembly and the annular ring so that the seal can protrude enough to align itself when pressurized,: . A2.2.2 Make the appropriate pneumatic connections, and adjust the pressure. A2.2.3 Initialize the system by nulling the force indicator and introducing a small amount ofgas in order to set the seat and align the device. A2.2.4 If the device is fully automated, select the desired . rate of load and set the mode switch to its run position; otherwise, manually control the gas pressure to the device so. that the rate ofstress does not exceed 150 psi/s (1 MPa/s) yet reaches its maximum within 100 s. A2.2.5 Record both the maximum pressure attaiiied and the appropriate force or stress multiplier for the specific detaching assembly. a stu, PNEUMATIC PISTON FIG. A2.1 SEMiero Pneumatic Adhesion Tester 796 DUP050297978 APPENDIX (Nonmandatory Information) XI. STRESS CALCULATION XI. 1 The stress computed in 8.2 is equal to the uniform uH-off strength of the analogous rigid coating system ifthe l ilied force is distributed uniformly over the critical locus the instant of failure. For any given continuous stress 'bution where the peak-to-mean stress ratio is known, uniform pull-off strength may be approximated as; U = XR .lore; .uniform pull-off strength, representing the greatest force that could be applied to the given surface area, psi (MPa), measured in-situ pull-off strength calculated in 8.2, psi , (or MPa) and ., ( -n peak-to-mean stress ratio. important to note that a difference between these -off strengths does not necessarily constitute an error; rather the in-situ measurement simply reflects the actual character of the applied coating system with respect to the analogous "ideal" rigid system. XI.2 An error is introduced if the alignment of the apparatus is not normal to the surface. An approximate correction by the peak-to-mean stress ratio is: R = (l + 0.14 az/d), where: z = distance from the surface to the first gimbal or the point at which the force and counter force are gener ated by the action of the driving mechanism, in. (mm), d = 'diameter of the loading fixture, in. (mm), a = angle of misalignment,' degrees (less than 5), and R = maximum pekk-to-mean stress ratio for the misaligned rigid system. The American Society for Testing and Materials fates no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, arid the risk of infringement of such rights, are entirely their own responsibly. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnotrevised, either reapproved or withdrawn. Your comments are Invitedeither forrevision of this standard orfor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive carefqi consideration at a meeting of the responsible technical committee, which you may. attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 1 797 DUP050297979 (jjjiM Designation: D 4563 - 86 (Reapproved 1991)e1 Standard Test Method for Determination by Atomic Absorption Spectroscopy of Titanium Dioxide Content of Pigments Recovered From Whole Paint1 This standard is issued under the fixed designation D 4563; .the number.immediately following the, designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates dn editorial change sirice'tlie last revision or reapproval. ** NYZ' --Keywords were added-editorially in February 1991. ' 1. Scope 1.1 This lest method covers the atomic absorption (AA) analysis of titanium dioxide content in pigments recovered frqm whole paint. It is applicable to quality control situa tions where the same type of product is repeatedly analyzed. 1.2 This standard dogs not, purport to. address the safety problems, if any, associatedyriih.its,use. It is'theresponsi bility of the user, of ifyis. standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7. . . .. 2. Referenced Documents 2.1 ASTM Standards:.. ;,v D 1193 Specification for Reagent-Water? t ,. D1394 Test Methods for Chemical Analysis of White ' Titanium Pigments13 * i E 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals4 E 288 Specification for Volumetric Flasks5 3. Significance and Use 3.1 This test method may be used in quality control laboratories when the repeated analysis of titanium dioxide in simitar paints may be required. Reagents and time are kept to a minimum when this test method is used in place of wet chemical analysis such as in Test Methods D 1394. However, reproducibility and repeatability are not as good as in Test Methods D 1394. 4. Summary of Test Method 4.1 The specimen is prepared for analysis by ashing at 450C followed by digestion with sulfuric acid and ammo 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D0J.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Jan. 31, 1986. Published March 1986. ~ Annual Book ofASTM Standards, Vols 06.03 and 11.01. 1 Annual Book ofASTM Standards, Vol 06.02. 4 Annual Book ofASTM Standards, Vol 15.05. 5 Annual Book ofASTM Standards, Vol 14.02. nium sulfate as in Methods D 1394. The titanium content ? ; determined by atomic absorption spectroscopy using th specimen similar to that previously analyzed by the AU( *" minum Reduction Method in Test Methods D 1394. 4.2 By utilizing the pigment analyzed in Test Methods i D 1394 as an atomic absorption standard, several hundre'df Ti02 determinations can be made. The AA technique much faster than the technique in Test Methods D 1394 I multiple determinations and' uses only acids. This ke.r reagents aiid time to a minimum.' 5. Apparatus 3.1 Atomic Absorption Spectrophotometer, consisting | 5.1.1 Atomizer and nitrous oxide burner, 1, ,5.1.2 Gas-pressure regulator, and metering devices fora nitrous oxide and acetylene, - 5.1,3'Titanium' hollow cathode lamp with regulated corojj sta'riit-curi'ent; supply, 5.1.4 Monochromator and associated optics, 5.1.5 Photosensitive detector connected to an electrc amplifier, 5.1.6 Readout device. | 5.2 Muffle FurnacCj- capable of maintaining 450 25 5.3 Circulating Oven, maintained at 105 2C. 5.4 Porcelain Dishes, 90-mm diameter. 5.5 Plastic Disposable Syringe, 10-mL capacity. 5.6 Agate Mortar and Pestle, 95-mm outside dianietei. 5.7 Wide-Mouth Erlenmeyer Flask, 500-mL capacity. 5.8 Hot Plate, with variable surface temperature control from 10"C above ambient to 370C accurate to within 5 <' ^ 5.9 Burner. 5.10 Volumetric Flask, 1000 mL, plastic (see Specification; E 288). 5.11 Paint Shaker. t! 5.12 Weighing Bottles, wide-mouth, with an externals fitting cap, and no larger than necessary for required amount of sample. 5.13 Desiccator. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall I used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chefflji 798 DUP050297980 D 4563 Society, where such specifications are available.6 Other Mtrades may be used, provided'it is first ascertained that the 11 .gent is of sufficient high purity to permit its use without feeing the accuracy of the determination. <jM2 Purity of Water--Unless otherwise indicated, !refer- iQfces to water shall be understood to mean reagent water ^/onforming to Type II of Specification Dll 93.' tjSfl.'i Ammonium Hydroxide (sp gr 0.90)--Concentrated ", onium hydroxide (NH,,OH). F 86.4' Ammonium Sulfate (NH4)2S04). fS.5 Hydrochloric Acid (sp gr 1.19)--Concentrated hydro- fcoric acid (HC1). ||.6 Hydrofluoric Acid (HF)--Approximately 49 %. |,7 Standard Pigment Solution. . 73X6.7.1 Following the procedure in Section 9 recover the JJgment from a! paint that is similar to the unknown jpeirnen. Analyze the extracted pigment for Ti02 content in 'ferdance'with the Aluminum Reduction Method in Test SRihods D 1394 and record the percent Ti02 foundin the Blent. . , JB.t.2 FOllowingthe procedurein 12.1 through 12.5 takea Igpiinen of the pigment extracted, in 6.7.1 into solution, lie this solution for no more than 3 months in a plastic Bggle marked with the percent Ti02 as determined in 6.7,1. f.8 Sulfuric Add (sp gr 1.84), concentrated, sulfuric acid po4). ,, ..,, S|i9 Toluene. , . . ,. ,, ,, jjHazards i >" 3 g.l Concentrated Hydrofluoric Acid--Make certain to ebserve manufacturer's recommended precautions for han||ng. p2 Warning--Nitrous oxide and acetylene can cause ^plosions, if not used properly. See the suppliers manual of juftructions for the atomic absorption instrument for proper deration with these gases. ^Calibration and Standardization Operational instructions for atomic absorption, fecuophotometeis vary With different models. Consult the Mtufacturer's literature for establishing optimum condijls for the specific instrument used. , , $s2 :Turn the instrument on and set the wavelength to the i5.3-nm titanium line..Apply the recommended Gurrent to $o titanium hollow cathode lamp. Allow the instrument to jfarm up for about , 15 min and set the proper, slit width.* Bust the gas: pressures and ignite the burner in accordance llpinstructions .for using, nitrous oxide and acetylene., J8.3 Aspirate, the water to rinse the atomizer chamber from jto 15 min,until the burner;head achieves temperature Koplibrium. Set the. instrument reading to zero, while doing ws. While aspirating'the working standard from 6,7.2 set the Jjfhsteument to the percent Ti02 (determined, in 6.7.1). |Ke.ispirate the water and reset the instrument to ZERO, ippeat this procedure until the readings become stable. _____ "Reagent Chemicals, American Chemical Society Specifications," Am. CbemiltSoc., Washington, DC. For suggestions on testing of reagents not listed by the 3jrlieriean Chemical Society, see "Reageni Chemicals and Standards" by Joseph D. Van Nostrand Co., Inc., New York, NY, and the "United States irmacopeia.' 8.3.1 Expanding the scale of a spectrophotometer in creases the noise level of the readout system. Therefore, if expanding the scale to make the readout indicate 60 % Ti02 has this effect, do not use any expansion. For instance, it is nOt necessary to make the instrument read 60 For 60 % Ti02 Standard. It may read 30. If 60 % equals 30,' a pigment giving a reading of 25 would have a TiOz content of 50 %. ' FIGMENT CONTENT 9. Procedure .i 9.1 Mix the samples until homogenous, preferably on a mechanical1 Shaker. If air bubbles become entrapped in the sample, stir by hand. 1 9.2 Draw approximately 5 g of the paint under test into a 10-mL Syringe arid weigh to 1 mg. Transfer, by dropwise addition, between 2.0 and 4.0 g of the specimen to a tared porcelain dish containing either 2 mL of water (for water borne paint) or 2 mL of toluene (for solvent-borne paint). ReWeigh-the syringe1 to.T mg. Swirl the dish during the addition- of the paint and continue to swirl until the specimen" is completely dispersed. -If a water-borne paint tends to agglomerate or form lumps that cannot be dispersed, a drop or two of concentrated NH4OH may help the dispersement. Ifthe lumps persist, discard the specimen, and prepare a new one. Prepare a duplicate specimen in the same mapner. ; ... , ,..3:,X>ry the specimens at H0*C for 30 min and then drive off the remaining solvent or water .at the lowest, temperature possible using a Maker burner (under a-hood). Do not. leave the dishes on the. burners after the flames have subsided. 9.4 Transfer the dried specimens tp a muffle furnace and heat at 450 ,25C for at. least 1 h and,until no further char is .evident. Leave.the furnace door slightly open after first inserting the dishes to allow smoke and possibly flames to escape raakipg certain the. furnace is well .vented. 9.5 Remove the dishes from the muffle furnace, cool in a desiccator,, and \yeigh. ., 9.6 Grind the pigment to passthrough,an 80-mesh screen. 10.Calculatjqn ..,... , 10.1 Calculate the percent pigment content as follows: Cw-W fx too where: P pigment content, % C - weight of the dish and specimen after ignition, g, W, - weight of the dish alone, g, W2 - specimen weight used, g. 11. Precision and Bias (see Practice E 180)7 11.1 In an'interlaboratory study of this test method in which operators in each of seven laboratories made duplicate analyses on different days and one operator in one laboratory made duplicate analyses on one day and a single analysis on the second day on a water-borne flat wall paint, a solvent- 7 Supporting data are available from ASTM Headquarters. Request RR: D01-1046. 799 II jy DUP050297981 # D 4563 borne semi-gloss enamel and a solvent-borne house paint containing 33, 38.5, and 37 % pigment, respectively, the pooled within-iaboratory standard deviation was found to be 0.07 % absolute with 21 df. The pooled between-laboratories standard deviation was 0.22 % absolute with 21 df. One laboratory's results for one day were discarded because the duplicates differed significantly and another laboratory's results for one day because the range differed significantly from all other ranges for Coating 1 and a third laboratory's results for one day because it differed significantly from the other day's results and those from all other laboratories for Coating 2. Based on these standard deviations the following criteria should be used forjudging the acceptability ofresults at the 95 % confidence level: 11.1.1 Repeatability--Two results, each the mean of du plicates, obtained by the same operator should be considered suspect if they differ by more than 0.21 % absolute at pigment contents of 33 to 39 wt %. 11.1.2 Reproducibility--Two results, each the mean of duplicates obtained by operators in different laboratories, should be considered suspect if they differ by more than 0.66 % absolute at the same pigment content levels. TITANIUM DIOXIDE CONTENT 12. Procedure 12.1 Determine the dry weight of two weighing bottles with caps. In accordance with Table 1 select the appropriate specimen weight and place the approximate! amount of recovered pigment in each weighing bottle. 12.2 Dry the specimens in the open weighing bottles for 2 h at 105C. Cool in a desiccator. After cooling, cap the weighing bottles and weigh as rapidly as possible. 12.3 Transfer the dry specimens to 500-mL wide-mouth Erlenmeyer flasks. Reweigh bottles and caps and record weights ofspecimens transferred (W4 in equation in 13.1 and 13.2). 12.4 To the 500-mL flasks, which now contain the specimens, add 8 g 0.001 g of (NH4)2S04, 50 mL of concentrated H2S04 and 5 drops of concentrated HN03. Mix well by swirling the flasks. Heat on a hot plate until dense white fumes are evolved. Continue heating over a hot flame until solutions are complete (usually requires not more than 5 min of boiling), or until it is apparent that the residues are composed of SiOz or siliceous matter. Cool and add 100 mL of water with extreme caution. TABLE 1 Specimen Weight Requirement Expected Ti02 on pigment, % Specimen Weight, mgA 0 to 19 20 to 29 30 to 39 40 to 49 50 to 59 60 to 69 70 to 79 80 to 89 90 to 100 1000 500 330 250 200 160 140 130 110 * Equivalent to about 60 ppm Ti in the final solution. 12.5 Quantitatively transfer the contents of the flanks including any insoluble matter to 1000-mL plastic volu metric flasks (see Specification E288). Add 50 mL of He I and 30 mL of HF. Allow to cool to room temperature av then fill to the mark with water. Stopper and mix well Transfer the solutions to plastic bottles (because of the Hfj and store for no more than 3 months for analysis by A \ Solutions must be filtered through a Whatman 42 paplt before being aspirated. 12.6 Calibrate the instrument in accordance with Section 8 and aspirate the solutions in the following order: 1--water (set to ZERO) 2--working standard (set to percent Ti02) 3--specimen (read) 1--water (set to ZERO) 2--working standard (set to percent Ti02) 3--specimen (read) This MUST be repeated until the readings are stable. 13. Calculation 13.1 Calculate the percent Ti02 in the pigment as follows' TiO,, CXW-, W4 where: C = reading of specimen (number 3 in 12.6), W3 = standard pigment weight in 6.7.1, g, and W4 = specimen pigment weight in 12.3, g. 13.2 Calculate the percent Ti02 in the whole paint a, follows: Tio2%,.i^ w4 where: A = pigment calculated in 10.1, %, and P, Wit and W4 = same as in 13.1. 14. Precision and Bias (see Practice E 180)7 14.1 In an interlaboratory study of this test method which operators in each of eight laboratories'analyzed different days a water-borne flat wall paint, a solvent-borne* semi-gloss enamel and a solvent-borne house paint, res\c tively containing 28.8, 56.8, and 42.8 weight % titaniu dioxide in the pigment, the pooled within-laboi. standard deviation was found to be 0.65 % absolute with degrees of freedom. The pooled between-labor; standard deviation was 1.31 % absolute with 20 degrees i freedom. One duplicate value from one laboratory discarded because the range differed significantly from other duplicate ranges for Coating 1, one day's result hot another laboratory because the range differed significantly) from all other ranges and both day's results from a third laboratory were discarded because the mean differed signi3{ cantly from all other laboratory means for Coating 2, and i one duplicate value was discarded from the same laboratory as with Coating 1 because the range differed sign from all other duplicate ranges for Coating 3, Based on these1* standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence^ level: ;* i 800 DUP0502 97982 # D 4563 1*14.1.1 Repeatability--Two results, each the mean of duates obtained by the same operator, should be considered -ect if they differ by more than 1.91 % absolute at TiC>2 , htents of 28 to 57 weight % of the pigment. ;4.1.2 Reproducibility--Two results, each the mean of implicates, obtained by operators in different laboratories should be considered suspect if they differ by more than 3.68 % absolute at the same levels of Ti02 content. 15. Keywords 15.1 atomic adsorption spectroscopy; percent pigment by ignition; titanium dioxide, analysis of The American Society lor Testing and Materials takes no position respecting tfie validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standardor for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. >-v., 801 DUP050297983 Designation: D 4584 - 86 (Reapproved 1991)e Standard Test Method for Measuring Apparent pH of Electrocoat Baths1 This standard is issued under the fixed designation D 4584; the number immediately following the designation indiiates the year of original adoption or, in the case of revision, the year oflast revision. A. number in parentheses indicates we year o PP superscript epsilon (<) indicates an editorial change since the last revision or reapproval. (` N[\' --Keywords were added editorially in January 1991. 1. Scope 1.1 This test method covers the measurement of the free hydrogen ion concentration of electrocoat baths and their ultrafiltrates. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water12 D 1293 Test Methods for pH of Water3 E 70 Test Method for pH of Aqueous Solutions with the Glass Electrode4 E ISO Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals4 3. Summary of Test Method 3.1 A specimen of a well-agitated electrocoat bath is placed in a stirrer-equipped container and the pH measured with a pH meter and associated glass and reference elec trodes. 4. Significance and Use 4.1 The pH is the measure of the free hydrogen ion concentration of a sample, and it indicates whether an electrocoat bath is acidic, neutral, or basic. Since pH measurements of good precision are made in aqueous solutions, it is suggested that the pH measurements of electrocoat baths are only semi-quantitative, and therefore such measurements should be referred to as apparent pH measurements. 4.2 The pH of electrocoat paints is used for research, production, and quality control or electrocoat bath process control. 4.3 Other related methods for determining the pH of water or aqueous systems are described in Test Methods D 1293 and E 70. 1 This test method is under the jurisdiction of ASTM Committee 1>1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved April 25, 1986- Published June !9S6. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01, 5 Annual Book ofASTM Standards, Vol 11.01. 4 Annual Book ofASTM Standards. Vol 15.05. 5. Apparatus 5.1 pH Meier, 5.2 Glass and Reference Electrodes. j I No t e--Due to the polarity of electrocoat materials it is desirabljj use a separate set of electrodes for each bath polarity, calhodic and'f anodic, because a bath of opposite polarity poisons the electrode.-. aM desired practice is to rinse the electrodes after each measurement with ' [, appropriate solvent for the electrocoat material, J 5.3 Thermometer, capable of 0.5C accuracy with a -2 to 1 32C range. 6. Reagents 6.1 Reference Standard Solutions, commercial standards,'1! of pH 4.0, 7.0, and 10.0. | 6.2 Purity of Water--References to water shall be under-'' stood to mean water conforming to Type II of Specification! D 1193. 1 7. Sampling and Sample Preparation 7.1 The sample should be obtained while the electrocoatl bath is under proper circulation so that a uniform material is i obtained. In case of an ultrafiltrate, the material should be 1 thoroughly mixed orstirred prior to sampling to assure, uniformity. s 7.2 After sampling and prior to removing a test specimf it is mandatory that the sample be shaken or stirred until if homogeneous and free of any settled material. This i; particularly important If there is any delay between T sampling of the bath and the preparation of the specime for the test. The absence of settled material can be ascsr-4 tained visually (in a transparent container) or by inserting spatula, scraping the bottom of the container to make sure1) that there is no settled matter. Shake or stir the samples unfit! specimens are taken for measurement; this point is re ! important. 8. Procedure 8.1 Standardization--Turn on the pH meter and allow ) to warm up. Wash the electrodes with a stream of water, the pH meter manufacturer's instructions to calibrate electrodes with buffer solutions of pH 4 and 7 for cationicl systems and 7 and 10 for anionic systems. Rinsing the1',* electrodes thoroughly after each calibration. The references!1 buffer solutions should thoroughly match the temperature bf?| the samples to be measured within 2C. j 5.2 Apparent pH Measurement: 8.2.1 Place a suitable quantity of a well-mixed eiectrocoajg specimen in a clean and dry container equipped with a stirrer (preferably magnetic). Operate the stirrer fast enough to' avoid separation of the paint but slow enough to prevent splashing or vortexing. Allow the temperature of the 802 DUP050297984 <H D 4584 ^pcimen to come to equilibrium (that is, the temperature 'ijbould show a drift of less than 0.5C/min). Record the jySnpcrature, and dial in the temperature correction on the J'Lpfl ineter. Place the electrodes in the specimen and deter mine the pH value in accordance with the pH meter jjHitoufacturer's instructions. Record the pH value and the ' liperature of the specimen. B |.2.2 Run two successive specimens of the electrocoat '""iSath sample; the pH value should be within 0.1 units/min jimi should show drifts of less than 0.1 units/min. If these fp limits are not met, check the pH meter and repeat the Bple procedure. &?|||fPrecision and Bias jjggp. 1 In an interlaboratory study of the test method, with imp laboratories naeasuring five electrocoat bath samples Syith pH ranging from 2.6 to 8.0, the intralaboratory Mpdard deviation (in accordance with Practice E 180) was found to be 0.03 units at 25 df, and the interlaboratory coefficient of variation was 0.08 units at 20 df. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 9.1.1 Repeatability--Two results, each the mean of dupli cate determinations, obtained by the same operator on different days should be considered suspect if they differ by more than 0.1 units. 9.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 0.3 units. 9.1.3 Bias--Bias cannot be determined for this test method. ID. Keywords 10.1 electrocoat baths, pH; pH measurement; ultrafil trates, pH The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in tftfe standard. Users of this standard are expressly adWsed that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reepprcvetfor withdrawn. Your comments are invited either forrevision ofthis standardor for additional standards and should be addressed to ASTM Headquarters. Ybur comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.. If you feel that your comments have not received a fair hearing you should mate your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. i * 803 DUP050297985 Designation: D 4585 - 87*1 Standard Practice for Testing Water Resistance of Coatings Using Controlled Condensation1 This standard is issued under the fixed designation D 4585; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. fl N]^' --Paragraph 7.3 was corrected editorially in June 1988. 1. Scope 1.1 This practice covers basic principles and operating procedures for testing water resistance of coatings using controlled condensation. Condensation is produced by ex posing one surface of a coated specimen to a heated, saturated mixture of air and water vapor, while the reverse side of the specimen is exposed to the cooling effect of room temperature air. This practice is derived from research of.thie Cleveland Society for Coatings Technology.2 1.2 This practice is limited to the methods of obtaining, measuring, and controlling conditions and procedures of controlled condensatidri tests. It does not specify specimen preparation, specific test conditions, or evaluation of results. N_`' 1--Alternative practices for testing water resistance of coatings include Practices D 870, D 1735, and D 2247. 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products3 D 610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces3 D714 Test Method for Evaluating Degree of Blistering Paints3 D823 Test Methods for Producing Filins of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D 870 Practice for Testing Water Resistance of Coatings Using Water Immersion3 * This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.27 on Accelerated Testing. Current edition approved Nov. 27, 1987, Published January 1988. Originally published as D 4585 - 86. Last previous edition D 4585 - 8fia. 2 Foecking, N. J., "Cleveland Condensing Type Humidity Cabinet,'' Officio! Digest, December 1963, Vol 35, No. 467, pp. 1318-1327; and Higgins. W, A., "Cleveland Condensing Type Humidity Cabinet: II," Official Digest, November 1965, Vol 37, No. 490, pp. 1392-1404. 3 Annual Book ofASTM Standards, Vol 06.01. D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting4 D1735 Practice for Testing Water Resistance of Coatings;* Using Water Fog Apparatus3 , D2247 Practice for Testing Water Resistance of Coatings!* In 100 % Relative Humidity3 D2616 Test Method for Evaluation of Visual Color 1 Difference With a Gray Scale5 6 D3359 Test Methods for Measuring Adhesion by Tapep! Test3 ,| D 3363 Test Method for Film Hardness by Pencil Test3 G53 Practice for Operating Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for' i Exposure of Nonmetallic Materials6 !i|| 3. Summary of Practice 3.1 Water vapor is generated by heating a pan of water aft the bottom of the test chamber. The specimens form the roof or walls of the test chamber so that the back sides of the i specimens are exposed to the cooling effects of root#*! temperature air. The resulting heat transfer causes vapor topi condense on the test specimens as liquid water saturated witlf|P air. 3.2 The temperature and amount of condensate forminfll on the specimens is controlled by the test temperature and1 the room temperature. The test specimens are inclined so' that condensate runs off the test surface by gravity and is replaced by fresh condensate in a continuous process during' the condensate cycle. 3.3 Exposure conditions are varied by selecting: (a) the temperature of the test, (b) the duration of the test, and (. periodic drying of the specimens. Testing may be conducted , j at temperatures from 100 to 180"F (38 to 82"C). Any effect|| such as color change, blistering, loss of adhesion, softening, :]! or embrittlement are observed and reported. 1 4. Significance and Use 4.1 Water can cause degradation of coatings, so knowl edge of how a coating resists water is helpful in predicting its service life. Failure in a condensation test may be caused by a number of factors including a deficiency in the coating itself, contamination of the substrate, or inadequate surface preparation. The test is therefore useful for evaluating 4 Annual Book ofASTM Standards, Vols 02.05 and 06.01. 5 Annual Book ofASTM Standards, Vol 14.02. 6 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 804 DU P050297986 # D 4585 FIG, 1 Controlled Condensation Apparatus ;co.rings alone or complete coating systems. 1 F'4-2 Condensation tests of coatings are used for specificaacceptance, quality control, and research and develop- Int of coatings and substrate treatments. These tests ptially result in a pass or fail determination but the degree of Blure also may be measured. A coating system is considered flpass if there is no evidence of water-related failure after a ratified period of time, ||i3 Results obtained from the use of condensation tests in liordance with this practice should not be represented as ling equivalent to a period of exposure to water in the est |tural environment, until the degree of quantitative corre- ;osurfi* |on has been established for the coating or coating system. ?) fori.. S.4 The test is usually conducted on metal or wood pecimens with the coating facing the inside of the chamber. Spwever, it is possible to test the blister resistance of house, gpits on wood specimens by mounting the uncoated wood Mir it e Kxit face facing the inside of the chamber. |jh5 This practice can be used for corrosion tests particu- of the JJly if the specimens are periodically dried. While corrosion :room ||oducts will drain into the water bath, they are not carried por to ` dwith'' hto the vapor that condenses on the test specimens. rromg e and ted so and is luring a) ;h, ;nd (<1 fueled effects Apparatus7 ; 5.1 Test Chamber (see Figs. 1 and 2), consisting of Bpsulated side walls mounted on a base, test specimen racks Kttached to the side walls, a heated water pan, and provisions j|>r controlling and indicating the vapor temperature within Kie chamber. Vents, approximately 0.10 to 0.20 in. (3 to 5 JSim) wide, shall be provided to admit room air at the bottom l|f the test chamber. 1 Nab' 2--The apparatus described in Practice G 53 may be used if |jhe ultraviolet lamps specified in Practice G 53 are turned off. filling, * j 5.2 Specimens shall form the roof of the test chamber. If Jphe specimens cannot completely fill all the openings, blank |janels shall be used. Specimens shall be inclined from 15 to |f5 from the horizontal and arranged so that condensate is inowl- greturned to the water pan without dripping on other speci- ing its fjoens. sed by oating 5.3 Water Supply, with water level control. 5.4 Water Heater, preferably located under the water pan, urface j controlled by a thermostat with the sensing element located uating fin the water. S- 5.5 Thermometer, with the stem extending into the air- 7 Apparatus from Q-Panel Co., 26200 First St,, Cleveland, OH <14145 has been found satisfactory for this purpose. Equivalent apparatus may be used. PIG. 2 Apparatus Cross Section water vapor mixture in the test chamber. , 5.6 Program Timer, Blower, and Air Heater, (optional) fitted to the chamber to provide periods of drying on a fixed schedule. 6. Test Specimens 6.1 This practice does not cover the preparation of test specimens. The substrate composition and surface prepara tion, specimen preparation, and the number of specimens should be agreed-upon prior to testing. Ncd' 3--Applicable methods for the.preparation of test panels and substrates are given in Methods D 609 and Practices D 1730. Test Methods D 823 cover application techniques for the production of uniform films. 7. Procedure 7.1 Fill the water pan tb a depth of approximately 1 in. (25 mm) with water. The quality ofthe water in the pan does not affect the test since the evaporation and condensation process yields distilled water, but the use of tap water can result in the accumulation of residues in the water pan. 7.2 Fill all spaces in the specimen holder rack with specimens or corrosion-resistant blank panels. Mount coated metal panels with the coating to be tested facing the inside of the chamber. Coated wood specimens may be mounted in the same way. 7.2.1 Blister tests to simulate the effects of water vapor migration from inside a frame house are mounted with the uncoated side of the wood specimen facing the inside of the test chamber. 7.2.2 Seal all cracks between specimens and holes in specimens with tape or metal strips. Condensate may seal small openings but cracks larger than 0.04 in. (1 mm) and holes larger than 0.08 in. (2 mm) in diameter can cause water vapor loss and local temperature variation. 7.3 Adjust the thermostat to maintain the desired temper ature of the saturated air and water vapor mixture. Vapor temperatures of 100, 120, or 140F (38, 49, or 60C) are suggested. Other temperatures may be used provided that the 805 DUP050297987 # D 4585 temperature is reported in conformance with Section 8. To ensure adequate condensation, maintain a 20F (HC) temperature differential between the room and the vapor. 7.4 Operate the chamber continuously unless otherwise specified or agreed. The removal of specimens for inspec tions during operation is permitted. When removing a specimen for inspection, replace it with a blank so that the test conditions are not altered. 7.5 Cyclic operation with alternating periods of condensa tion and drying may be used. Automatic drying requires the apparatus described in 5.6. For manual drying of specimens, remove them from the apparatus. Drying periods should be at least 4 h long. 7.6 Conclude the test after a specified period of time or after effects from exposure to water are noted. 7.7 Remove specimens at the conclusion of the test; Do not leave the; specimens in the apparatus at the conclusion of the test as the specimens can remain wet for hours, or even days, when the apparatus is turned off. 7.8 Wipe the test specimens dry. Rate specimens for changes in color, blistering, etc. Evaluate specimens no less than 5 min and no more than 10 min after removal from test, as the effects from water exposure can change within a short time. Remove only as many specimens as can be rated within the specified time. Nef' 4--The 0 to 10 scale described in ASTM STP 500s >s Preferred for rating. Relevant procedures for evaluating water effects are describM in Methods D 610 and D 2616, and Test Methods D 714, D 3359 a, D 3363. 7.8.1 If possible, rate the specimens again after they have been removed from the test for a recovery period long enough that moisture absorbed within the specimen dries out and the specimens reach moisture equilibrium with room : air. A recovery period from 12 to 24 h is generally sufficient. ! The post-recovery rating allows evaluation of the permanent effects of the exposure as distinct from the transient effects, and is especially important for evaluation of color and glos, 8. Report 8.1 Report the following information: 8.1.1 Sample identification. 1 8.1.2 Results of the evaluation(s). i 8.1.3 Reference to Practice D 4585. 8.1.4 Hours of test duration. j 8.1.5 Description of any cyclic operations. j 8.1.6 Condensation temperature. | 8.1.7 Special conditions of test or anydeviations in testi procedure. ail 8 Paint Testing Manual. ASTM STP 500, ASTM, 1972- Tha American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, and the risk of Infringement ot such rights, are entirely their own responsibility. This standard Is subject to revision ,af any time by the responsible technical committee end must be reviewedevery five years and if net revised, either reapproved or withdrawn. Your comments are Invited either torrevision of this standard or toradditional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting ot the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASJM Commlttee on Standards, 1916 Race St, Philadelphia, PA 19103. 806 DUPO 502 97988 M Designation: D 4587 - 91 erred ribed . arw Standard Practice for lave Conducting Tests on Paint and Related Coatings and ng out otn Materials Using a Fluorescent UV-Condensation Light- and Water-Exposure Apparatus1 eni lent This standard is issued under the fixed designation D 4587; the number immediately following the designation indicates the year of cts. original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A OSS superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 4'ttpe tllfi Tbis practice covers the selection of test conditions Practice G 53 to be employed for exposure testing of ||and related coatings and materials. This standard does not purport to address all of the w,problems associated with its use. It is the responsibility fuser ofthis standard to establish appropriate safety and il'h practices and determine the applicability of regulatory est WrdJtions prior to use. Inferenced Documents ASTM Standards: 358 Specification for Wood to Be Used As Panels in ^feathering Tests of Coatings2 23 Test Method for Specular Gloss2 '09 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 SlO Test Method for Evaluating Degree of Rusting on painted Steel Surfaces2 1559 Method of Evaluating Degree of Chalking of Exterior Paints2 660 Test Method for Evaluating Degree of Checking of Exterior Paints2 lljpfil Test Method for Evaluating Degree of Cracking of ||[|gyExterior Paints2 j|Bp)62 Test Method for Evaluating Degree of Erosion of IjjExterior Paints2 ;1 Bf714 Test Method for Evaluating Degree of Blistering of Rpaints2 $772 Test Method for Evaluating Degree of Flaking K.(Scaling) of Exterior Paints2 j|:823 Test Methods for Producing Films of Uniform {Thickness of Paint, Varnish, and Related Products on {{Test Panels2 IjjjlOOS Test Methods for Measurement of Dry Film iThickness of Organic Coatings Using Micrometers2 U.86 Test Methods for Nondestructive Measurement of { Dry Film Thickness of Nonmagnetic Coatings Applied *Bto a Ferrous Base2 i|;i400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 If^iiThis practice is under the jurisdiction of ASTM Committee D-l on Faint and feted Coatings and Materials and is the direct responsibility of Subcommittee s^P1.27 on Accelerated Testing. Current edition approved Feb. 22, 1991. Published April 1991. Originally llrshed as D 4587 - 86. Last previous edition D 4587 - 86. fAnnual Bonk of ASTM Standards, Vol 06.01. D1654 Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive Environments2 D1729 Practice for Visual Evaluation of Color Differences of Opaque Materials3 D1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting4 D1731 Practices for Preparation of Hot-Dip Aluminum Surfaces for Painting4 D1732 Practices for Preparation of Magnesium Alloy Surfaces for Painting4 D2092 Practice for Preparation of Zinc-Coated (Galva nized) Steel Surfaces for Painting2 D2244 Test Method for Calculation of Color Differences from Instrumentally Measured Color Coordinates2 D2616 Test Method for Evaluation of Visual Color Difference With a Gray Scale5 D 4214 Test Methods for Evaluating Degree ofChalking of Exterior Paint Films2 E 97 Test Method for Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter' Reflectometry5 G53 Practice for Operating Light- and Water-Exposure Apparatus (Fluorescent UV-Condensation Type) for Exposure of Nonmetallic Materials5 3. Significance and Use >'. 3.1 Organic coatings on exterior exposure are subjected to attack by degrading elements of the weather, particularly ultraviolet light, oxygen, and water. This practice may be used for evaluating the behavior of films exposed in appa ratus that produces ultraviolet radiation, high temperatures, and water condensation on the films. This apparatus is used to make an early materials comparison of the exterior exposure quality of paints. However, light sources, such as the fluorescent UV lamp, that emit a significant amount of radiation at wavelengths shorter than those in natural sunlight, may cause results that lead to unrealistic evalua tions of weathering properties. 3.2 As no single light exposure apparatus, with or without water, can be specified as a direct simulation of natural exposure, this practice does not imply expressly, or other wise, a specific correlation with outdoor exposure. It has, however, been useful in many instances. 3.3 Since climatic conditions vary with respect to time. * Annual Book ofASTM Standards. Vol 14.02. 4 Annual Book ofASTM Standards, Vols 02.05 and 06.01. * Annual Book ofASTM Standards. Vols 06.01 and 14.02. 807 DUP050297989 0 4587 geography, and topography, it may be expected that the effects of natural exposure will vary accordingly. All mate rials are not affected equally by the same environment. Results obtained by use of this practice should not be represented as equivalent to those of any outdoor weathering test unless the degree of quantitative correlation has been established for the material in question. 3.4 Variations in results may be expected when operating conditions among similar type instruments vary within accepted limits of this standard procedure. 4. Test Specimens 4.1 Unless otherwise agreed upon, choose panels that meet the applicable base panel requirements specified in Standards D 358, D609, D 1730, D 1731, D 1732, or D 2092, Select panel sizes suitable for exhibiting the failure mode to be observed. 4.2 Apply the coatings to flat panels with the base panel material, method of application, coating system, film thick ness, and method of drying consistent with the anticipated end use, or as mutually agreed upon between the producer and the user. If it's not possible to testflat samples, you may need to take special precautions to ensure that {!) the sample holders seal behind the samples so that the water vapor does not escape from the test chamber, and (2) the closest part of the samples to the UV lamps is at the 50-mm distance specified in Practice G 53. If part of the sample is closer to the lamps, it will be subject to more intense UV exposure. 4.3 Unless otherwise agreed upon, coat test panels in accordance with Test Methods D 823 and measure the film thickness in accordance with an appropriate procedure selected from Test Methods D 1005, D 1186, or D 1400. Nondestructive methods arc preferred because panels so measured do not need to be repaired. 4.4 Unless otherwise specified, before exposing coated panels in the apparatus, condition them at 73.5 3.5? (23 2C) and 50 5 % relative humidity for one of the following periods in accordance with the type of coating: Baked coatings Radiation-cured coatings All other coatings 24 h 24 li ? days minimum 5. Apparatus 5.1 Fluorescent UV/Condensation Apparatus, complying with Practice G 53.6 6. Procedure 6.1 Place panels within the 8.25 by 35.35-in. (210 by 900-mm) area as described in Practice G 53. Reposition the panels on a regular schedule as described in Practice G 53 to minimize any effects from temperature or UV light varia tion. When the test specimens do not completely fill the racks, fill the empty spaces with blank non-rusting panels to maintain the test conditions within the chamber. 6.2 Use the test conditions specified by mutual consent or required by a product quality specification. Some test conditions in current use for testing paint and related & Apparatus and lamps from Q-Panel Co., 26200 First St., Cleveland. OH 44145 and from Atlas Electric Devices Co., 4114 N. Ravenswood Ave., Chicago. IL 606! 3, have been found suitable for this purpose. coatings and materials are: A = 8 h UV/70C followed by 4 h CON/50C for automo- five coatings, B -- 4 h UV/60C followed by 4 h CON/50C for general metal coatings, C = 4 h UV/6CPC followed by 20 h CON/60C for exterior wood coatings, D -- 8 h UV/60C followed by 4 h CON/45C for industrial maintenance coatings, E = other test temperatures and time cycles that conform to the Procedure section of Practice G 53. where: UV = ultraviolet light (lamps) only, and CON = condensation conditions only. Ngh' 1--Temperatures are black panel temperatures measured in the panel rack. 6.3 Program the selected test conditions and operate the apparatus continuously within the limits specified in Practice G 53. Service the apparatus in accordance with Practice G 53. Nij' 2--Variations in results can occur as the result of not changing lamps in accordance with the manufacturer's instructions. 7. Periods of Exposure 7.1 Use one of the following methods to determine the duration of the exposure under this practice: 7.1.1 A mutually agreed upon specified number of total hours. 7.1.2 The number of total hours of exposure required to produce a mutually agreed upon amount of change in either the test specimen or an agreed upon standard sample. 8. Evaluation of Results 8.1 Evaluate conditions of exposed test specimens by means of one or more of the following standards: D 523, D 610, D 659, D 660, D 661, D 662, D 714, D 772, D 1654, D 1729, D 2244, D 2616, D 4214 and E 97. Select methods in accordance with product use requirements. 8.2 Because of possible variations in results as described in 3.4, no reference should be made to results obtained from tests conducted in the apparatus using this practice unless! accompanied by Section 9 or unless otherwise specified in a] reference procedure. 9. Report 9.1 Report the following information: 9.1.1 Manufacturer and model of fluorescent UV/> condensation apparatus. 9.1.2. Manufacturer's designation for the fluorescent UV: lamp and the relative spectral energy distribution of the, lamp. This may be accomplished by listing the manu facturer's designation, wavelength (nm) where peak emission; occurs, and the wavelength near low cut-off where 1 % of peak emission occurs. 9.1.3 Exposure cycle, for example, 4 h UV/60"C. 4 h. CON/50"C. 9.1.4 Total exposure time. 9.1.5 Results of panel evaluation (see 8.1). 9.1.6 Identification of standard used for comparative evaluation, if any. DUP0502 97990 # D 4587 The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In thts standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you fee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 809 DUP0502 97991 Designation: D 4610 - 86 Standard Guide for Determining the Presence of and Removing Microbial (Fungal or Algal) Growth on Paint and Related Coatings1 This standard is issued under the fixed designation D46I0; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (*) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This guide describes techniques used for determining the presence of fungal or algal growth on paint and related coatings and methods for removal of such growth prior to recoating. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and heath practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D2022 Method for Sampling and Chemical Analysis of Chlorine-Containing Bleaches2 D3274 Test Method for Evaluating Degree of Surface Disfigurement of Paint Films by Microbial (Fungal or Algal) Growth or Soil and Dirt Accumulation3 3. Significance and Use 3.1 Microbial growth is a major cause ofdiscoloration and deterioration of paint films. This guide describes techniques used to distinguish fungi and algae from other surface contaminants. 3.2 Repainting a surface contaminated with fungi or algae generally causes more rapid infestation of the new paint than repainting a surface from which fungal or algal growth has been removed. This guide describes methods for removing fungal or algal growth prior to repainting. 4. Reagents 4.1 Sodium Hypochlorite, approximately 5 % aqueous (NaOCl) as commercial household bleach. Because sodium hypochlorite decomposes on exposure to heat and sunlight and becomes ineffective, use only fresh material. See Method D 2022 for methods of sampling and chemical analysis. 4.2 Trisodium Phosphate, or non-ammonia-containing laundry detergent. 1 This guide is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.28 on Biodeterioration. Current edition approved Aug. 29, 1986. Published October 1986. 2 Annua! Book ofASTM Standards, Vol 15.04. 1 Annual Book oj ASTM Standards, Vol 06.01. 5. Procedures 5.1 Determining the Presence of Fungal or Algal Growth on Paint: 5.1.1 Chemical--Apply a drop of 5 % aqueous sodiu r. hypochlorite solution (common household bleach) to the area suspected of being contaminated with fungal or algal growth. Fungal or algal discoloration will normally bleach within 60 s. Discoloration that does not bleach is probably dirt. For further confirmation do visual and subculture tests. 5.1.2 The following procedures should preferably be used by persons who have had basic microbiological training: 5.1.2.1 Visual--Examine the surface using magnification from 10 to I00X to distinguish among fungal, algal, or dirt disfigurement in accordance with Test Method D 3274. 5.1.2.2 Subculture--Apply a prepared petri dish con taining a raised convex surface of nutrient agar culture medium4 directly to the surface to be sampled and exert moderate pressure. Replace the cover and incubate for least 72 h at 95"F (35C). Examine the agar surface visualc. as in 5.1.2.1. Nkl' t--The culture medium must contain the nutrients necessary for growth of algae and fungi. 5.2 Removal ofFungal and Algal Growth on Paint: 5.2.1 Wash the surface with a solution of approximately 5 % trisodium phosphate in water or a solution at approxi mately 2 % laundry detergent in water. 5.2.2 Thoroughly rinse the surface with water to remove residual trisodium phosphate or detergent. 5.2.3 Wash the surface with a solution of 1 part by volume of sodium hypochlorite 5 % aqueous solution and 3 parts by volume of water. Nmn' 2--The solution should be allowed to remain on the surface from 10 to 15 min. Nop' 3--The sodium hypochlorite solution and the 2 % laundry detergent solution may be combined 1:1 by volume in one treatment t desired. 5.2.4 Thoroughly rinse the surface with water to remove residual sodium hypochlorite. 5.2.5 If agreed upon by the parties involved, reinspect the surface in accordance with 5.1 to ensure that there has been adequate removal. Refer to the coating manufacturerliterature for recommended drying time before recoating. 4 Agar available from BBL Microbiology Systems, Div. or Becton, Dickinson and Co., P.O. Box 243, Cockeysvilie, MD 21030 or Scott Laboratories, It Fiskcvillc, RI 02823, has been found suitable for this purpose. 810 DU P 0502 97992 0 D4610 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Yourcomments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments vfriH receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race Si, Philadelphia, PA 19103. DUP050297993 Designation: D 4618 - 87 Standard Specification for Design and Fabrication of Flue Gas Desulfurization System Components for Protective Lining Application1 This standard is issued under the fixed designation D 4618; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This specification covers the design and fabrication of metal components for Flue Gas Desulfurization (FGD) equipment, including absorbers, tanks, chimney liners, ductwork and associated equipment that are to be lined for corrosion or abrasion resistance, or both. 1.2 Limitations--This specification does not cover struc tural performance of FGD components. It is intended only to define the design considerations for successful application and performance of protective linings for FGD system components. 1.3 This specification represents the minimum require ments for lining work. In cases where the manufacturer's instructions and recommendations differ from this specifica tion, these differences must be resolved before fabrication is started. 1.4 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information only. 1.5 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Design/Engineering Requirements 2.1 Rigidity: 2.1.1 The components shall be designed so that the interior metal surfaces are sufficiently rigid for the intended lining materials. Manufacturer's recommendations for max imum strains or deflection limits for the lining material shall be followed. 2.1.2 The weight of the lining system shall be considered in the structural design of the component. 2.1.3 The design shall consider the effects of pressure, wind, seismic and other design loads. 2.1.4 Vibration may cause flexing or high surface strains on the lining. This is of particular concern to rigid lining materials and shall be minimized. 2.1.5 Special consideration shall be given to all areas of potentially excessive strain such as unsupported bottom areas, oil-canning, out of roundness, sidewall-to-bottom joints, etc. J This specification is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.09 on Protective Linings for FGD Systems. Current edition approved Feb. 20, 1987. Published April 1987. 2.1.5.1 Where a component is on a concrete foundation grouting shall be done if necessary to correct unsupported bottom areas. 2.1.5.2 Sand fill shall not be used for bottom suppo.i unless provisions are made to assure that the sand cannot be lost due to erosion. 2.2 Accessibility: 2.2.1 All interior surfaces of the components shall be designed to be readily accessible for surface preparation and lining application. 2.2. L1 All fillets and corners shall be accessible for proper welding and grinding. 2.2.2 The minimum manway size for a working entrant r. during lining application shall be 36 in. (900 ram) m diameter or 24 in. (600 mm) width by 36 in. (900 mmj height. 2.2.2.1 Closed components shall have a minimum of two manways, one near the top and one near the bottom preferably located 180 apart to facilitate adequate ventila tion for workers. 2.2.2.2 Additional or larger openings may be required lo facilitate ventilation and material handling. The lining mate rial applicator should be consulted for specific requirements.' 2.3 Shell Penetrations: 2.3.1 All connections or openings in the vessel or compo nent shall be flush with the interior wall. Inlet nozzle shall' extend into vessels if incoming fluids can be detrimental lo lining materials. Any exterior or interior connection shall be flanged in order to facilitate linings. 2.3.2 The maximum length of flanged nozzles, 4 in. (10IJ mm) and greater in diameter, shall not exceed the dimen sions in Table 1. 2.3.2.1 Only 4 in. (100 mm) diameter and larger nozzles shall be used for maximum reliability of the lining system. 23.2.2 As an alternative to lined nozzles, compatible prefabricated, reinforced plastic, ceramic or alloy metm inserts (sleeves) may be used if they offer superior corrosion and abrasion protection. Lining shall overlap onto prefabri cated liners. TABLE 1 Maximum Length of Nozzles Nominal Nozzle Size, in. (mm) Maximum Nozzle Length-- Shell to Face of Flange, in. (mm) 4(100) 6(150) 8-24 (200-600) 24-36 (600-900) Over 36 (900) 8 (200) 12 (300) 16 (400) 24 (600) any length 812 DUP050297994 D 4618 ndation, ipporled suppurt annot be shall be tion jr'i propei 3.3 Lining thickness may dictate changes in nozzle the temperature of the element. usions to achieve design flow rates. 2.4.4 Special precautions shall be taken in lined compo Appurtenances Inside Components: nents where severe abrasion/impingement damage may jj|4.1 The requirements in Sections 2 and 3 apply to any occur. Precautionary design measures, such as wear plates, rtenances that are being lined and installed inside a brick liners or added coating thickness, shall be considered component, such as agitators, anti-swirl baffles, gaging when necessary. :es, internal piping, ladders, and support brackets. 2.5 Structural Reinforcement Members and Supports: ,4.2 If appurtenances inside the component cannot be 2.5.1 Structural reinforcement members (stiffeners) shall p, they shall be made of corrosion-resistant materials. If be installed on the vessel exterior, wherever necessary. J' are used, the lining shall carry over the welded area However, if such members are installed internally they shall -torn! le alloy a minimum of 3 in. (76 mm). Some linings be fabricated of simple closed shapes such as round bars, 'ofay require special designs to protect the edge of the lining, pipe, or box beams for ease of applying the lining material. iiluiolted connections are used, dielectric insulation shall be 2.5.2 The use ofbox beams or pipe for internal supports is frijjvided. 2.4.3 Heating elements shall be attached with a minimum |ance of 6 in. (150 mm) from the surface of the lined jtonent. Greater clearance may be required to protect the hmitg from excessive temperature conditions depending on recommended. The use of angles, channels, I-beams and other complex shapes shall be avoided wherever possible. If they must be installed internally, these members shall be fully seal welded and the edges ground to a '/ in. (3 mm) minimum radius. 2.5.3 If closed chambers are formed with internal box beams or pipes, they shall be vented to the atmosphere at the BUTT WELD (A-Acceptable, B&C-Unacceptable) lowest point, so that pressures are not developed during operation and possible curing procedures and so that corro sion, due to localized lining failures, can be observed early. enhance irm) in 00 irm) n of to b >tlum ' ventilai- i/a- (3<nm| MAX. 3. Fabrication 3.1 Welds: 3.1.1 Ail internal welds to be lined shall be continuous without imperfections such as weid slag, weld splatter, rough surfaces, undercutting, high peaks, porosity, sharp corners, sharp edges and inadequate thickness (see Fig. 1). 3.1.2 The degree of weld preparation prior to lining depends on the type of lining to be applied. The lining manufacturer must be consulted for specific requirements for weld preparation during the design ofthe component and prior to start of fabrication. 3.1.3 Use of weld display samples before and after grinding may be of help to the component fabricator in supplying acceptable welds with a minimum required re work. All welds shall be inspected prior to lining. Whenever possible, shop welds shall be inspected in the fabricator's shop. 3.1.3.1 AH weld areas shall be inspected before and after blast cleaning, Pinholes, pits, blind holes, porosity, undercut ting or similar depressions are not permissible in the finished surface. 3.1.4 Weld splatter shall be removed. Chipping' may be utilized only if followed by grinding for the required surface finish. 3.1.4.1 The use of non-silicone, anti-splatter coating ap plied adjacent to weld areas is suggested. This coating shall be of a type that can be removed by the final blast cleaning. 3.1.5 After inspection, all undercuts and pinholes shall be eliminated by welding or grinding. All rough welds shall be ground to remove sharp edges. Chipping may be used to remove sharp edges if followed by grinding. 3.1.6 All edges and similar abrupt contours shall be rounded off by grinding or machining to a '/s-in. (3 mm) minimum radius. 3.1.7 Fillets and changes in contour shall be ground to a `/s-in. (3-mm) minimum radius where required for the selected lining material. Any grinding done on welds, edges, 813 DUPO 502 97995 BOLTED FLANGE JOINT ALLOY FLANGE JOINT t-3-H //---IINWG -CARBON STEEL uu -SUITABLE GASSET BETWEEN UNEO FLANGES WELDED FLANGE JOINT CONTIM/OUS WU> J----SURFACE TO BE ON0 -SUITABLE GASKET - STITCH OSCONTIMCOUS WELD FIG. 2 Joint Fabrication for Lining Application and fillets shall be done carefully to eliminate potential problems caused by gouging of the parent metal. 3.1.8 All internal and external welding shall be completed prior to any lining application. 3.2 Joints: 3.2.1 All welds shall be continuous. Intermittent or spot welding is not permitted (see Fig. 2). 3.2.2 Riveted joints shall not be used. Internal bolted joints shall not be used except to avoid welding on an already lined surface. In this case, corrosion resistant alloy or nonmetallic bolts shall be used. 3.2.3 If bolts are used to facilitate installation or welding, or both, of a component, they shall be removed and holes plug welded before lining application. 3.2.4 Lap welded joints shall be avoided whenever pos sible. Where they are necessary, the interior lap shall be a full fillet weld and finished as in accordance with 3.1.6. 3.2.5 Expansion joints and bolted flanged duct or shell joints require special lining consideration. Bolted flange joint surfaces shall be lined before assembly. Special consideration shall be given during erection and fit-up so as not to damage the lining. 3.2.5.1 If alloy flanges are used at expansion joints, the design must allow for the lining system to be applied over the alloy by 3 in. (75 mm). Some linings may require special designs to protect the leading edge. 3.3 During and after the lining of the equipment, no welding shall be allowed on the interior or exterior surfaces. 3.4 Signs shall be hung or stenciled on the exterior surface of the equipment designating the following: LINED EQUIP MENT, DO NOT BURN OR WELD. They shall be visible from all elevations and sides of the equipment. 4. Drawing Notes 4.1 All lined surfaces should be clearly identified on all detail and arrangement drawings. DOUBLE LAP JOINT CONTINUOUS WELD SURFACE TO QS LINGO - U2- (36MM) MIN. CONTINUOUS OR STITCH WILD CRIMP^OINT SURFACE TO 81 LINED - CONTNUOUS WELD - // I- CONTINUOUS OR STITCH WGO FIG. 2 (Continued) Joint Fabrication for Lining Application 4.2 The following note shall appear on appropriate detail and arrangement drawings: All surfaces to be lined shal meet the requirements of ASTM Specification D 4618. 814 DUP050297996 # D 4618 CORNER JOINTS SURFACE 10 HE LINED SURFACE TO BE LINED - STITCH OB CONTINUOUS WELD SURFACE t o BE LINED--/ CONTINUOUS WELO --^ *_ STITCH OR CONTINUOUS WE.D FIG. 2 (Continued) Joint Fabrication for Lining Application The American.Society for Testing end Materials takas no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to retfsfbn at any time by the responsible technical committee and must be reviewed every five years and if riot revised, either reapprovedor withdrawn. Yourcomments are invited either for revision ofthis standard or for additional standards and should be addressed to AS7M Headquarters. Your comments will receive careful consideration at a meeting of the responsible ' technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.; Philadelphia, PA 19103. 815 DUP050297997 Designation: D 4619 - 91 Standard Practice for Inspection of Linings in Operating Flue Gas Desulfurization Systems1 pec This standard is issued under the fixed designation D46I9; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or rcapproval. 1. Scope 1.1 This practice describes procedures for conducting inspections of the conditions of various linings in operating Flue Gas Desulfurization (FGD) system components. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. For specific hazard statements, see Section 7. 2. Significance and Use 2.1 Periodic inspections are essential to evaluate lining performance, to detect existing damage potential problems, and to plan scheduled maintenance. The frequency of these inspections may diminish or increase with time depending upon lining performance. 3. Recordkeeping 3.1 Lining condition will depend on the operating condi tions experienced by the lining systems. Records of these conditions that are maintained by the owner/operator should be evaluated for potential effects upon the linings. These may include: 3.1.1 Dates of lining installation and initial operation, 3.1.2 Solution/gas temperatures in lined components, 3.1.3 Solution/gas chemistry (pH, composition), 3.1.4 Start up/shut down dates, 3.1.5 Gas velocities and particulate loading, and 3.1.6 Ambient conditions. 3.2 Any known change in the process criteria or modifi cations of the physical design shall be identified and dated. 3.3 All past history pertaining to the lining systems should be available during the inspection process. They may in clude: 3.3.1 Copies of existing lining specifications and installa tion procedures. 3.3.2 Quality control documents of the existing lining installation. 3.3.3 Copies of previous inspection reports. 3.3.4 Documentation pertaining to any maintenance of existing lining systems. 1This practice is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.09 on Protective Linings for FGD Systems. Current edition approved Aug. 15, 1991. Published October 1991. Originally published as D 4619 - 86. l ast previous edition D 4619 - 86. 4. Inspection Team 4.1 The owner/operator should select a team of experi enced personnel to conduct the inspection. Personnel repre senting the following may be included: 4.1.1 Owner's representative, 4.1.2 Lining manufacturer, 4.1.3 Lining applicator, 4.1.4 Equipment designer, 4.1.5 Architect engineer, 4.1.6 Third party inspectors, and 4.1.7 System designer. 5. Pre-Inspection Procedure ; Ss 5.1 Prior to conducting an inspection of the lining, the < owner/operator shall ensure that the following services and ! equipment are provided. . f 5.1.1 Safety--The inspection team shall verify that the : equipment being inspected has been made safe for entry. ' This shall include lockout procedures for related equipment " such as, but not limited to, the boiler, dampers, valves, fans, and pumps. Ji 5.1.2 Lighting--Sufficient lighting shall be provided to . assure general lighting of the overall area plus localized high ' intensity lights for close visual observation or taking ot photographs, or both. The lighting fixtures shall be equipped with a safety guard to nfinimize breakage and injury. ill 5.1.3 Access to Lining Surfaces--The access equipment j must meet all safety requirements of OSHA and the owi operator. The equipment must he capable of placing inspectors close enough to the lining surface to perform all inspection procedures. 5.1.4 Cleaning--Selected lining surfaces to be inspectfij shall be cleaned of any deposits or buildup that will obsculjj examination of the lining. The cleaning procedure selectej must not cause damage to the lining. ' 'ijj 5.1.5 Ventilation--Provisions must be made to . > that adequate fresh air is provided in all FGD components^ being inspected. If some components are on line, provisioljl must be taken to adequately isolate such components. 6. Hazards TM 6.1 All safety requirements of OSHA and the owner/'j| operator, must be met when performing all inspection# operations. Residues, including acids, heavy metals, or othpj hazardous materials, may be present in deposits, on tij^j lining surfaces, or in the atmosphere. Precautions shall BW taken to protect personnel. Confined entry safety requit8| ments shall be adhered to where applicable. 816 DU P0502 97998 Inspection Procedures 8.2.2 Date(s) of inspection, 7.1 The inspection should include visual examination, otographic examination, mapping of potential problem reas, specific destructive or nondestructive testing, and Kpaoval (if required) of representative samples for analysis Be Table I). 8.2.3 Participants and their affiliation, 8.2.4 Documentation of inspection, 8.2.5 Photographs, as applicable, 8.2.6 Mapping of problem areas, 8.2.7 Test results, and _ |;7.2 Temperature may influence observed or tested lining I(.(parameters, such as crack width, hardness, and adhesion, 'qhuring inspection, temperature of the lining surface and the 8.2.8 Conclusions and recommendations. 9. Repairs liniterior and exterior ambient temperatures of the compo- 9.1 If repairs of the lining are required, the owner/oper hint should be measured and recorded. ator or his representative shall prepare specific repair specifi ; jsk,7.3 Other parameters important to the inspection should cations or procedures, or both, with the input of the lining f (discussed with the parties involved and agreed to prior to Ien- g inspection. manufacturers), the applicator(s), and others as necessary. 9.2 These specifications or procedures, or both, may be prepared in advance or as a result of the inspection. {Report ' 8.1 The owner/operator shall designate who is responsible 10. Keywords _yi;ir the preparation of an inspection report. 8.2 Report the following information: 10.1 cementitious linings; chemical resistant linings; flue gas desulfurization (FGD); inorganic linings; inspection of 8.2.1 Pertinent background information contained in Sec- linings; organic linings; power generation facility linings in 3, Organic Resins inspection: Igpiist gphemicai Degradation Jpt/rtace Effects: Up, Abrasion/erosion pi Aligatoring/checking Discoloration/charring ' ^-"Flaking ijjgJlOracking gjpiSoftening '^STratering/deiamination: g'llSize [fjpiDensity V.l ^Entrapped contents for analysis Hi Mechanical Damage |fijpsfca/ Testing: '^pi'ing thickness Continuity testing of suspect areas, (confirm test voltage with lining Bpu- manufacturer) . s.'plhesion testing, if required . \ il TABLE 1 Lining Maintenance Inspection Parameters Organic Elastomers . Inorganic/Cementitious Visual Inspection: Rust Chemical Degradation Surface Effects: Abrasion/erosion Swelling Softenin'g Crazing Cracking Surface sloughing Blistering: Size Density Entrapped contents for analysis Mechanical Damage: Gouging Cutting Tearing Overcbmpression {mating sur- faces) Adhesive failure Cohesive failures Reversion (Reverting to soft con ditions with loss of physical properties) Physical Testing: Lining thickness Continuity testing of suspect areas, (confirm test voltage with lining manufacturer) Adhesion testing, if required Shore durometer hardness Visual inspection: Erosion/mechanical damage Cracking Softening Spalling Rust staining Efflorescence Anchor exposure Delaminations Substrate exposure Physical Testing: Hardness {Schmidt hammer) Measure crack widths and pattern Core samples, if required Remove cementitious layer to permit visual examination of under- %v laying membrane/substrate > Inorganic/Masonry Visual Inspection: Erosion/mechanical damage Cracking: Mortar joint Brick face Spaltng Softening: Brick Mortar Expansion joint Color Change: Brick Mortar Physical Testing: Hardness (Schmidt hammer) Core samples, if required Petrographic analysis, if required The American Society for Testing and Materials takes no position respecting the validity of any patent rights assertad in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited efther forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Pace Sf., Philadelphia, PA 19103. 817 DUP050297999 i Designation: D 4707 - 87 (Reapproved 1991} Standard Test Method for Measuring Pairit Spatter Resistance to Roller Application1 This standard is issued under the fixed designation D 4707; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflastreapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the tendency of a paint to spatter when applied with a paint roller to a substrate. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and heath practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 3924 Specification for Standard Environment for Con-' ditioning and Testing Paint, Varnish, Lacquer, and Related Materials2 D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 2.2 Other Document: Photographic Standards of Paint Roller Spatter3 3. Summary of Test Method 3.1 The test paint is applied to a black plastic panel by draw-down. The coated plastic panel is immediately mounted on an essentially vertical surface above a sheet of paper used to catch any spatter. A specially designed notched spool roller (see 5.1) is rolled through the film following a defined procedure, tending to generate spatter. Any spatter falls upon the spatter catch paper, and after drying is rated against the photographic standards. 4. Significance and Use 4.1 Paint spatter generated by roller application is depen dent on the properties of both the paint being applied and the paint roller cover used for the application. To eliminate the influence of the paint roller cover as a variable, and thus restrict the spatter-inducing variable to the paint under test only, the paint roller cover is replaced by a standard notched spool roller to generate spatter by a mechanism that simu lates that of a paint-applying roller cover. 4.2 Although most of the development work to establish this test method was undertaken using latex paints, sufficient work was also done to show its applicability to solventreducible paints. 4.3 Tests during the development of this test method showed that the spattering properties of paints, like other physical properties, may in time change. Therefore, ihj results ofthis test are valid only for the time when the test is run. 5. Apparatus 5.1 Notched Spool Test Roller (Fig. I).4 5.2 Glass Plate, at least 9 by 19 in. (230 by 485 mm) by 'A in. (6 mm) thick. 5.3 U-shaped Film Caster,5 having a 7-mit (175-um) clearance by 5`A in. (135 mm) wide. 5.4 Mechanical Metronome, with swinging arm. 6. Materials 6.1 Black Plastic Panels,6 6Vz by 17 in. (165 by 430 mm).,j 6.2 Flannel Cloth. 6.3 Masking Tape, 1 in. (25 mm) wide. 6.4 Spatter Catch Paper, 18 by 18 in. (455 by 455 mm). 1 This paper can be any convenient paper to which the spattd droplets will adhere and of a color to contrast with the color of the paint under test. 7. Sampling and Conditioning 7.1 Sample the material in accordance with Practice D 3925. 7.2 Prior to testing, the samples shall be conditioned in: accordance with the standard atmosphere described in Speed" ification D 3924. The testing shall take place under the same , conditions. 8. Procedure 8.1 Clean the top of the glass plate and both sides of t black plastic panel to ensure that they are free of spo Place the black plastic panel on the glass plate and tape 1 narrow end at the top to the glass plate. Smooth the p- n along the plate to ensure a close fit. 8.2 Stir the paint under test thoroughly and strain toJ remove all skins and particles. Place the film caster with the ( ` This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D0I.42 on Architectural Finishes. Current edition approved May 29, 1987. Published July 1987. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Copies of the pictorial photographic reference standards are contained in Pictorial Standards of Coalings Defects and may be obtained from the Federation of Societies For Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. 4 The E-Z Paintr Notched Spool Test Roller, obtainable from the PrcciS'Otf ^ Gage and Tool Co., 28 Volkenand Ave., Dayton, OH 45410, has been found suitable for this purpose. 5 The Dow film caster, available from BYK-Gardner, Inc., Gardner Labors^ tory, 2435 Unden Lane, Silver Spring, MD 20910, has been found suitable for tnls purpose. 6 Leneta P-121-1 ON dull black plastic panels 6V> by 17 in. by 10 (production tolerance: 1 mil) (165 by 432 by 250 pm) in size, obtainable from th** Leneta Co., P.O. Box 86, Ho-Ho-Kus, NJ 07423, are suitable for the purpcsi. 818 DU PO 50298000 SPOOL MUST TURN FREELY # D 4707 A <| TOTAL ASSEMBLY (DIMENSIONS NOT CRITICAL) Dimensions A Flange thickness 8 Space between flanges C Total, cjlameter D Diameter under notches E. Hole diameter in. 0.063 0.005 0.343 0.005 1.600 0.015 1.400 0.015 0.261 0.005 FIG. 1 Notched Spool Roller mm 1.60 0.13 8.71 0.13 40.16 0.38 35.56 0.38 7.14 0.13 .O-mil (175-pm) side down immediately below the taped n|ion of the black plastic panel. Turn on the metronome, sljusted for 80 beats/min. Into the well formed by the film caster, pour sufficient paint so that the well is filled from jrner to comer. Draw down the paint the full length of the 'plastic panel, until the film caster is fully beyond the tredge. The rate of application should be fairly slow, 3 to 4 rom end to end, to prevent pinholes or holidays in the t film. .3 Immediately upon completion of the draw-down, emove the black plastic panel from the glass plate, keeping masking tape intact, and tape, with the long direction rtical, to a surface that is vertical or nearly vertical (within tpf vertical, top sloping away from the operator) with the ttom of the black plastic panel about 1 in. (25 mm) above e laboratory bench or table (Fig. 2). It is desirable that the urface under the black plastic panel be firm but with a little .silience. A backing of 'A-in. (6-mm) thick pasted iberboard7 is ideal as very hard surfaces make proper rfomtance of the test difficult. Center the spatter catch Iper on the laboratory bench or table under the black lastic panel. 7 Upson or universal board, manufactured by Domtar Gypsum Co., P. O. Box 508, Lockport, NY 14094, and available at most lumberyards, lias been found Suitable for this purpose. 8.4 Using the clean, notched spool roller, start in one of the upper comers and roll downward and upward through the paint film. Always keep,the notched spool in contact with the black plastic panel, fiot removing the roller from the film when changing directions. Make ten passes in each direction (20 passes total), 15 Vi in. (380 15 mm) per pass, progressively moving sideways from one edge of the film to the other (Fig. 3). Each pass should coincide with a beat of the metronome and the motion should be contin uous, not jerky. Try to emulate the motion of the metro nome, using the metronome for accurate timing (practice the motion with the metronome to gain the necessary rhythm and timing), since the speed of the rolling of the notched spool roller through the paint film has been found to be the only variable significantly affecting the results of the test. Make sure that all four flanges ofthe notched spool roller are within the draw-down area at all times. Use sufficient pressure to maintain constant contact between the notched spool roller and the black plastic panel. Note that as long as constant contact is maintained, pressure variations have not been found to noticeably affect the results. 8.5 Remove the spatter catch paper and lay it in a suitable place to dry. 8.6 Repeat the test with a second plastic pane! after cleaning the apparatus. 819 tmesi DUP050298001 D 4707 DRA'dDOWN AREA 9. Grading Procedure 9.1 Carefully cut an area 7J/2 by 9*/z in. (190 by 240 mm) out of the front edge (edge nearest the paint) of the spatter catch paper. The 7'/2-in. side will be the front edge. Center the area with respect to the spatter so a maximum of spatter is on this sheet (Fig. 4). 9.2 Using the photographic standards numbered I, 3,5,7, and 9 for comparison, rate each test with a number from 0 (low spatter resistance) to 10 (no spatter), interpolating as needed for ratings 2, 4, 6, and 8. Nqr' --Figures 5 through 9 are duplications thereof for sample purposes, not meant to be used for test grading purposes. 9.3 In rating the paints using the photographic standards, consider the population of spatter droplets of greater impor tance than the average size of the spatter droplets. 9.4 If the ratings of two tests do not agree within 1 unit, repeat until such precision is obtained. 10. Precision and Bias 10.1 A precision and bias statement is in development. 11. Keywords 11.1 paint spatter resistance; resistance--paint spatter; roller application; spattering Dimensions in. A Notched spool pass length B Drawdown width (determined by blade) C Panel width D Panel length 15 Vi 5Va 6Y2 17 FIG. 3 Test Pattern Schematic Jy Jrf! 11 3&0 - 1= * ? 140 >ffj 165 ,dL 430 "ill FRONT (Edge nearest to the owuntod panel during test.) 90]--? in. <l nm)-->| FIG, 4 Cutting Out Section of Spatter Catch paper for Evaluation 820 DUP050298002 i i DUP050298003 D 4707 DUP050298004 DUP0502 98005 D 4707 DUP050298006  j. # D 4707 fi. ?$ k i J1 825 DU P050298007 D 4707 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standardare expressly advised that determination of the validity of any such patent rights, and the, risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invitedeither forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 826 DUP050298008 Designation: D 4708- 91 Standard Practice for Preparation of Uniform Free Films of Organic Coatings1 This standard is issued under the Fixed designation D 4708; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {) indicates an editorial change since the last revision or reapproval. ^iScope [ This practice covers the preparation of free films of \Jire-fflic coatings for use in determining the physical proper- -i:Of the coatings. Procedures are given for preparing Free on four alternative substrates. These substrates are foil, treated FEP (fluorinated ethylene-propylene) et, silicone coated paper, and halo-silane coated glass Res. p.2 This standard does not purport to address all of the Wfy problems, if any; associated with its use. It is the fpbnsibility ofthe User ofthis standard to establish appro bate safety and health practices and determine the applicamy ofregulatory limitations prior to use, A specific hazard --lent is given in 6.1. ^Referenced Documents j|l ASTM Standards: jp> 823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels* . - ) 1005 Test Methods for Measurement of Dry-Film i Thickness of Organic Coatings Using Micrometers2 #>1653 Test Methods for Water Vapor Permeability of % Organic. Coating Films2 . *D2370 Test Method for Tensile Properties of Organic Coatings2 Summary of Test Method fl.l Free, films are prepared by depositing a uniform wet *ating of the test material on a release substrate. The plied films are dried or baked, cut into appropriate Size for le intended physical property test, and then stripped from e release substrate. ^Significance and Use 4.1 Free films are required for conducting tests to evaluate e tensile properties (Test Method D2370) and moisture gapor permeability (Test Methods D 1653) of organic coatis, 1.2 The tin foil/mercuiy amalgamation procedure should s used only in cases where FEP and paper substrates cannot ccommodate wetting or high-temperature baking condi- {This practice is under the jurisdiction of ASTM Committee D-l on Paint and Pfeiated Coalings and Materials and is the direct responsibility of Subcommittee '|j .23 on Physical Properties of Applied Paint Filins. Current edition approved Sept 15, 1991. Published November 1991. Originally Wished as D 4708 - 87. Last previous edition D 4708 - 87. 3Annual Book ofASTM Standards, Vol 06.01. 5. Apparatus 5.1 Equipment, for applying films of uniform thickness as described in Test Methods D 823. 5.2 Micrometer Film Thiclcness Gage, as described in Test Methods D 1005. 5.3 Alternative Release Substrates: 5.3.1 Dental Tin Foil, preferably 1-mil (25-gm) thick.3 5.3.2 Sheet of FEP,4 preferably 2-mils (50-pm) thick, coated with a thin film of a dry lubricant.5 5.3.3 Sheet of Silicone Coated Paper, preferably 5-mil (125-pm) thick.6 7 5.3.4 Glass Plates, coated with halo-silane compound. 5.4 Precision Specimen Cutter, having a double blade with a foot to hold the sample.2 Nst' 1--Other substrates that may be suitable are 10-mil (250-gm) thick polyethylene, photographic paper, polished steel, and fluoropolymer coated metal panels. 6. Hazards 6.1 Mercury--This practice involves the use of an OSHAdesignated hazardous substance, mercury. For information on the potential hazards and guidance relative to use, consult the supplier's Material Safety Data Sheet Mercury is a toxic metallic liquid. Its vapors are extremely hazardous. Small amounts of spilled mercury can vaporize sufficiently at room temperature to exceed the TVL of the vapor. Use with adequate ventilation (in a hood) or wear a respirator, and clean up spills immediately. Wear gloves when handling mercury. Containers should be kept closed. Droplets of mercury can be picked up by using a small glass pipe! connected to a suction flask with a rubber hose. 7. Procedure 7.1 Prepare the free films by one of the following proce dures: 7.1.1 Dental Tin Foil Substrate: 7.1.1.1 Apply each material to be tested to a strip of 3 Dental tin foil available from Yates and Bird, Chicago, 1L 60610 has been found suitable for this purpose. 4 Teflon FEP 2-mii film thickness (Card No, 03111, Item #29499) available from E.I. du Pont de Nemours & Co., Inc., Wilmington, DE 19898, has been found suitable for this purpose. 5 Dry lubricant (MS-122 Fluorocarbon Release Agent) available from MillerStcphcnson Chemical Co., Danbury, CT 06810, has been found suitable for this purpose. 6 Silicone coated release paper Form RP-1K, size 8J/a by 11 lA in., available from the l>.neta Co., P.O. Box 86. Ho-Ho-Kus, NJ, has been found suitable for this purpose. 7 The JDC Precision Sample Cutter manufactured by Thwing-Albert Instru ment Co., 10960 Dutton Rd., Philadelphia, PA 19154, has been found suitable for this purpose. 827 i DU P0502 98009 D 4708 dental tin foil. First, mount the foil on a smooth glass plate 7.1.2 FEP Substrate: a on which there may be placed a small pool of high-boiling 7.1.2.1 Apply each material to be tested to a treated sheet liquid. Spread the foil out to a smooth flat surface by means of FEP. First, cover a smooth, flat polished glass plate with a of a rubber squeege, which may be useful in holding the foil sheet of FEP. Coat the sheet uniformly with a light coat of a in close contact with the glass. Apply a uniform wet film of dry fluoro-carbon lubricant and allow to dry for 24 h at the material to the foil by one of the procedures given in Test standard conditions. Then apply a uniform wet coating of Methods D 823. Nuv' 2--Use a liquid that is known to have tittle or no effect on the test coating. In many eases a light mineral oil would be suitable. No t ' 3: Caution--Exercise care at all times to prevent the high- boiling liquids used in mounting the foil from coming in contact with the test film as these liquids may soften the film. For instance, the foil should be cleaned before amalgamation since any liquid remaining on the test material on the sheet by one of the procedures given in Test Methods D 823. 7.1.2.2 Dry the applied films in 73.5 3.5F (23 2"C) and 50 5 % humidity, or bake under conditions mutually agreeable to the producer and the user. Dry film thicknesses must not vary by more than the specified or agreed upon tolerances of the average film thickness and must be free of r*- the back of the foil and the test film will float on the bath of mercury. visible flaws. Most films with a thickness of less than 2.0 mil 7.1.1.2 Dry the applied films at 73.5 3.5"F (23 2C) and 50 5 % relative humidity, or bake under conditions mutually agreeable to the producer and the user. Dry film thicknesses must not vary by more than the specified or agreed-upon tolerance of the average film thickness and must not contain visible flaws. Most films with a thickness of less than 2.0 mil (50 pm) are very difficult to handle. 7.1.1.3 When required for further treatment such as weathering, remount the coated foil on a convenient smooth, flat substrate such as a glass or steel panel. In this case, a high boiling liquid (Note 2) may be used to hold the foil in close contact with the substrate over extended periods of time. 7.1.1.4 Age or expose the coated foil to conditions mutu ally agreed upon. At the end of the specified or agreed upon period, remove the foil-backed film from the glass or metal substrate and cut the specimens to size using a sharp knife or a precision specimen cutter. (50 pm) are very difficult to handle. 7.1.2.3 When required for further treatment such as weathering, remount the coated sheet on a convenient smooth, flat substrate such as a glass or steel panel. 7.1.2.4 Age or expose the coated sheet to conditions1 mutually agreed upon. At the end of the aging or exposure period, remove the sheet-backed film from the glass or rtu ta substrate and cut the specimens to size using a sharp knife the precision cutter (Note 4). Carefully strip the coating film from the sheet substrate. 7.1.3 Silicone Coated Paper: 7.1.3.1 Apply each material to a sheet of silicone coau paper. First, cover a smooth, flat substrate with a sheet of a silicone-coated release paper. Then apply a film of Ihe material under test, dry or cure, expose or treat if requir'd and prepare test specimens as described in 7.1,2 7.1.4 Halo-silane Coated Glass Plates--Apply each mate rial to a glass plate coated with a halo-silane compound. Nwx' 4--To prepare specimens for tensile property tests a precision specimen cutter must be used to ensure nick-free edges on the Specimens. Even with this instrument, it is necessary to cut each specimen independently, allowing at least 'h in. (50 mm) of waste First, coat a glass plate with a thin film of a halo-silane compound and dry.`Then apply a film of the material und test, dry or cure, expose or treat if required, and prepare test, specimens as described in 7.1.2. between specimens. 8. Keywords 7.1.1.5 Place the foil-backed specimen film side up on a pool of mercury to remove the foil by amalgamation. After amalgamation is completed, pick up an end of the floating film with tweezers, and carefully brush the unsupported film free of mercury and amalgam with a soft camel hair brush. 8.1 dental tin foil substrate; film; halo-silane coated glass plates; lacquer; organic coatings; paints and related coatings; polyhexafluoropylene (FEP) substrate; silicone-coated paper; substrates; surface preparation; tension (tensile) properties^ tests; vapors; varnishes The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, end the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration af a meeting of the responsible technical committee, which you may attend If you fee/ tfiaf your comment have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., P/?/7ade/pZi/a, PA 19103. 828 DUP050298010 Designation: D 4712 - 87a (Reapproved 1991) Standard Guide for Testing industrial Water-Reducible Coatings1 This standard is issued under the fixed designation D4712; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. Scope |i 1. 1 This guide covers the selection and use of procedures |r testing water-reducible coatings, both pigmented and liar, utilizing synthetic latices, synthetic resin emulsions, or 'ater-reducible alkyds. The methods included are listed in able 1. Where more than one standard is listed for the same haracteristic, no attempt is made to indicate superiority of je standard over another. Selection of the standards to be ilowed must be governed by experience and the requireients in each individual case, together with agreement itween producer and user. 1.2 This guide covers the testing of liquid coatings as iplied by conventional spray, airless spray, electrostatic itay, dip, fancoat, flowcoat, roller coat, and curtain coat. 1.3 This guide includes procedures relating to proper and ie packaging, shipping and receiving, and storage and idling during use and application. 1.4 This standard does not purport to address all of the kty problems, if any, associated with its use. It is the _ onsibility ofthe user ofthis standard to establish appro bate safety and health practices and determine the applica'ity ofregulatory limitations prior to use. 2. Referenced Documents `2.1 ASTM Standards: B 117 Metttbd of Salt Spray (Fog) Testing2 ' B 287 Method of Acetic Acid-Salt Spray (Fog) Testing3 D 16 Definitions of Terms Relating to Paint, Varnish, Lacquer, and Related Products4 'D 56 Test Method for Flash Point by Tag Closed Tester5 P;D 93 Test Methods for Flash Point by Pehsky-Martens Closed Tester6 D 185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints7 * D 344 Test Method for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts8 sD522 Test Method for Mandrel Bend Test of Attached ' Organic Coatings8 D523 Test Method for Specular Gloss8 This guide is under the jurisdiction of ASTM Committee D-l on Paint and jjplated Coatings and Materials and is the direct responsibility of Subcommittee ' .55 on Factory-Applied Coatings on Preformed Products. ?:- Current edition approved June 26 and Oct. 30, 1987. Published December Bf$87. |:. 2 Annual Book ofASTM Standards, Vols 03.02 and 06.01. r 3 Discontinued; See 1988 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 5 Annual Book ofASTM Standards, Vols 05.01 and 06.03. 6Annual Book ofASTM Standards, Vols 05.01. 7 Annual Book ofASTM Standards, Vols 06.01 and 06.02. ^ 8 Annual Book ofASTM Standards, Vols 06.01. ? 829 D 562 Test Method for Consistency of Paints Using the Stormer Viscometer8 D609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, lacquer, and Related Products8 D610 Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces8 D 658 Test Method for Abrasion Resistance of Organic Coatings by the Air Blast Abrasive8 D659 Method for Evaluating Degree of Chalking of Exterior Paints8 D660 Test Method for Evaluating Degree of Checking of Exterior Paints8 D661 Test Method for Evaluating Degree of Cracking of Exterior Paints8 D 662 Test Method for Evaluating P.egree of Erosion of , Exterior Paints8 D 714 Test Method for Evaluating Degree of Blistering of Paints8 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints8 D 822 Practice for Conducting Tests on Paint and Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light- and Water-Exposure Apparatus8 D 823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels8 D 869 Test Method for Evaluating Degree of Settling of Paint8 .. D870 Practice for Testing Water Resistance of Coatings Using Water Immersion8 D968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive8 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers8 D1014 Method for Conducting Exterior Exposure Tests of Paints on Steel8 D1125 Test Methods for Electrical Conductivity and Resistivity of Water9 D1150 Single and Multi-Panel Forms for Recording Results of Exposure Tests of Paints8 D1186 Test Methods for Nondestructive Measurement of Dry-Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base8 D 1200 Test Method for Viscosity by Ford Viscosity Cup8 D1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems8 D1212 Methods for Measurement of Wet Film Thickness of Organic Coatings8 9 Annual Book ofASTM Standards, Vol. lt.01. DUP050298011 # D 4712 D 1308 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes8 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness Df Nonductive Coatings Applied to a Nonferrous Metal Base8 ' D 1474 Test Method for Indentation Hardness of Organic Coatings8 i D1475 Test Method for Density of Paint, Varnish, Lac quers and Related Products8 D 1535 Test Method for Specifying Color by the Munsell System50 D 1540 Practice for Effect of Chemical Agents on Organic Finishes Used in the Transportation Industry8 D 1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature8 D 1653 Test Method for Water Vapor Permeability of Organic Coating Films8 D1654 Method for Evaluation of Painted or Coated ' Specimens Subjected to Corrosive Environments8 D 1729 Practice for Visual Evaluation of Color Differences of Opaque Materials10 D 1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting11 D1731 Practices for Preparation of Hot-Dip Aluminum `Surfaces for Painting1-1': D1732 Practices for Preparation of Magnesium Alloy ' Surfaces for Painting11 ' D 1735 Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus8 D 1737 Test Method for Elongation of Attached1 Organic Coatings with1 Cylindrical Mandrel Apparatus3 D 1848 Classification for Reporting Paint Film Failures Characteristic of Exteri or Latex Paints8 D 1849 Test Method for Package Stability of Paint8 D 2091 Test Method for Print Resistance of Lacquers8 D2092 Practice for Preparation of Zinc-Coated (Galva nised) Steel Surfaces for Painting8 D2196 Test Methods for Rheological Properties of Non- Newtonian Materials by Rotational' ' (Brookfield) Viscometer8 ' `' D 2197 T6St Methods for Adhesion of Organic Coatings by Scrape Adhesion8 D2201 Test Method for Preparation Of Hot-Dipped Nonpassivated Galvanized Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products8 D2243 Test Method for Freeze-Thaw Resistance of Wa- ter-Borrie Paints8 D2244 Test Method for Calculation of Color Differences from Iiistrumentally Measured Color Coordinates8 ' D 2246 Test Method for Finishes on Primed Metallic Substrates for Humidity-Thermal Cycle Cracking8 D2247 Practice for Testing Water Resistance of Coatings in 100 % Relative Humidity8 D2248 Practice for Detergent Resistance of Organic Finishes8 D 2353 Test Method for Flow Ratings of Organic Coatings Using the Shell Flow Comparator8 D2354 Test Method for Minimum Film Formation Tern perature (MFT) of Emulsion Vehicles12 D2369 Test Method for Volatile Content of Coatings8 D2371 Test Method for Pigment Content of Solvent. Reducible Paints8 D2454 Practice for Determining the Effect of Overbakin', on Organic Coatings8 D 2574 Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms8 D2616 Test Method for Evaluation of Visual Color Difference With a Gray Scale10 D2691 Test Methods for Microscopical Measurement of Dry-Film Thickness of Coatings on Wood Products8 D2697 Test Method for Volume Nonvolatile Matter in Clear*or Pigmented Coatings8 D2794 Test Methbd for Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact)8 .t D 2803 Test Method for Filiform Corrosion Resistance^1! Orgaiiic Coatings on' Metal8 ' D2805 Test Method for Hiding Power of Paints b> Redeclometry8 D2933 Test Method for Corrosion Resistance of Coated Steel Specimens (Cyelic Method)8 D 3002 Practice for Evaluation of Coatings for Plastics8* D3023 Practice for Determination of Resistance of Fat- tory-Applied Coatings on Wood Products to Stains and Reagents8 ` D 3134 Practice for Evaluating Color and Gloss Tol erances10 1 '' D3168 Practice for the Qualitative Identification of Pol) mers in Emulsion Paints7 D3170 Test Method for Chipping Resistance of Coatings8 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus13 D 3281 Test Method for Formability of Attached Organic Coatings with Impact-Wedge Bend Apparatus8 D3359 Test Methods for Measuring Adhesion by Tape Test8 D3361 Practice for Operating Light- and V/ater-Exposure Apparatus (Unfiltered Open-Flame Carbon-Arc for Testing Paint, Varnish, Lacquer, and Related Pr, j- ucts Using the Dew Cycle8 D 3793 Test Method for Low-Temperature Coalescence oi Latex Paint Films8 . :D3924 Specification for Standard Environment for Con ditioning and Testing Paint, Varnish, Lacquer, and Related Materials3 - D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings8 D3928 Test Method for Evaluation of Gloss or Sheen Uniformity8 D4060 Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser8 D 4062 Test Method for Leveling of Paints by Draw-Down Method8 D4399 Method for Measuring Electrical Conductivity of Electrocoat Baths8 45! P Re .m M Sr A 'He* hn 1H ii I "i 11 10 Annua! Book ofASTM Standards, Vol 14.02. 11 Annual Book ofASTM Standards, Vols 02.05 ami 06.01. 12 Annual Book ofASTM Standards, Vol 06.02. 13 Annual Book ofASTM Standards, Vol 06.03. 830 DUP050298012 ----------------------------------------- ----------------------------------------- I |` #'.D 4712 |i... Jp4585 Practice for Testing Water Resistanceof Coatings 8.J.8 Storage, variables, for example storage time, exces Z_ Using Controlled Condensation8 sive temperature fluctuations that may cause physical or P45S7 Practice for Conducting Tests on Paint and chemical change. Special needs arise due to carbon dioxide Related Coatings and Materials Using a Fluorescent absorption, dissolved metal compatibility, and ultrafiltration jj UV-Condensation Light- and Water-Exposure Appa- treatments. ratus8 B: 70 Test Method for pH of Aqueous Solutions with the , Glass Electrode1,4 |.2 U.S. Federal Test Method Standard No. 14led5 1131.1 Application of Sprayed Films |0! 1.2 Condition in Container 9. Liquid Coatings Properties , 9. i Condition in Container--Thickening, settling, and separation are undesirable and objectionable if a liquid coating cannot be reconditioned and made suitable for application with a reasonable amount of stirring. The j| Terminology referenced method covers procedures for determining ptl Definitions: l|i 1.1 For definitions of terms used in this guide, refer to gfinitions D 16. changes in properties after storage. Determine the condition in the Container in accordance with Method 3011.1 of US. Federal Test Method Standard No. 141c. 9.2 Coarse Particles and Foreign Matter--To form uni , Significance and Use form films of good appearance, the liquid coating must be (4:1 This compilation of standards is intended to provide sistance in selecting appropriate tests for evaluating water- ducible coatings and for determining what characteristics quid be considered for a given end use. Either single-coat |erations or multicoat systems may be addressed by the ffjper selection of tests. Results from the various tests are ; itt all necessarily useful in evaluating the performance of Iferent systems for various end uses. The list can be useful 1 !'those developing coatings and coating systems and to lose seeking coating systems for products. , free of coarse particles as agreed upon between the producer and the user, a typical maximum being I % by weight of the total paint. Determine coarse particles and foreign matter in accordance with Test Methods D 185. 9.3 Density or Weight Per Gallon--The density as mea sured by weight per gallon is used to help assure product' Uniformity from batch to batch. . In ' the referenced test method, the density is expressed as the weight in pounds avoirdupois of 1 U.S. gal or the weight in kilograms ofs l L of the paint at a specified temperature. A calibrated weigfttper-gallon cup is used. Determine the density in accordance s. Equipment ;J>,1 Use the equipment as specified in each standard. with Test Method D 1475. 9.4-Fineness ofDispersion--The more finely a pigment is dispersed, the more efficiently it is being used. One test /General Requirements jtr.l Tests and observations shall be at standard laboratory gnditions as specified in Specification D 3924 unless otherHjje specified or agreed upon by the producer and user. method for measuring the degree of dispersion (commonly referred to as "fineness of grind") is to draw the material down a calibrated, tapered groove in a hardened steel block with the groove, varying in depth from 4 to 0 mils (100 to 0 pm). The point at which continuous groupings ofparticles or T, Sampling and Specimen Preparation j/7.1 Sample the water-reducible coatings in accordance S'ith Practice D 3925. if.2 Prepare specimens as required for the specific tests on |e liquid coating and the dry coating. agglomerates, or both, protrude through the surface of the /'liquid is taken as the fineness reading. Lower readings in mils or pm or higher readings in Hegmah units indicate better fineness of dispersion. Determine fineness of dispersion in accordance with Test Method D 1210. 9.5 Pigment Suspension--The amount and type of set 8, Conditions Affecting Performance ;8.1 Practical requirements and performance of water- EJducible coatings may vary with: 8.1.1 Type of substrate. | 3S-L2 Substrate condition, for example, porosity, hard iness, smoothness, flexibility, etc. P 8.1.3 Type, quality, and suitability of the surface trfeatftrfent or primer used under the water-reducible coating and Hie time before coating application. 8.1.4 Application methods and techniques. 8.1.5 Contaminants on the surface of the substrate. 8.1.6 Environmental conditions such as temperature and ilclative humidity. 8.1.7 Damage to container, size, and type of container. tling is an indication of how well the pigments remain in suspension and how easily settled pigment can be remixed. Determine degree ofsettling in accordance with Test Method D 869. 9:6 Viscosity--Viscosity refers to the flow resistance of a flujd and should fail within an agreed-upon range. Viscosities of Newtonian fluids (constant viscosity regardless of shear rate) may be measured with a Ford Cup. Viscosities of non-Newtonian materials should be measured at two or more speeds with a Brookfield rotational viscometer. Deter mine viscosity in accordance with Test Methods D 1200 or D 2196. 9.71 Consistency--Consistency is a less precise term than viscosity for evaluating the flow properties of a material. In the referenced test method, consistency is defined as the load . in grams required to produce a specific rate of rotation in a 14 Annual Book ofASTM Standards, Vol 15.05. >. 1154Available from Standardization Documents Order Desk, Bldg. 4 Section D. '700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. specimen using the Stormer Viscometer. This is a one-speed test method and is not recommended for paints that show shear thinning or thixotropy. Determine consistency in 831 DUP050298013 Test Method I. Ugwtf Coating Properties: Coarse particles and foreign matter Condition in container Conductivity Consistency Density or weight per gallon Fineness of dispersion Rash point Freeze-thaw stability Microorganism resistance pH Package stability Pigment suspension Surface tension Viscosity 11. Application and Film Formation: Pane) preparation Drying properties Leveling properties Low temperature coalescence Spray properties Touch-up Uniform film preparation Wet film thickness Hi. /Appearance of Dry Film; Color difference by visual evaluation Color difference by instrumental evaluation Color description by visual evaluation Color description by Instrumental evaluation Gloss Hiding pov/er IV. Properties of Dry Film: Abrasion resistance Adhesion Elongation Exterior exposure Blistering Chalking Checking Cracking Erosion Flaking Rusting Accelerated weathering Corrosive environments Hardness Impact resistance Resistance to various forms of water Water immersion Water fog Humidity resistance Moisture vapor permeability Salt spray Humidity-thermal cycling Filiform corrosion Condensation Oetergent resistance Resistance to chemicals Overbaking Print resistance Reporting results Dry film thickness V. Analysis of Paint: Volatile content Volume of nonvolatile Weight of nonvolatile Pigment content Identification of vehicle solids # D 4712 TABLE 1 Section 9 9.2 9.1 9.14 9.7 9.3 9.4 9.13 95 9.11 9.8 9.10 95 9.12 9.6 List of Test Methods by Properties ASTM Standard D 185 D 1125 or 04399 D 562 D 1475 D1210 D 56. D 93 or 0 3278 D2243 D2574 E 70 01849 D 869 D1200 or D 2196 10 10.1 105.2 10.3 10.5 10.2.1 10.6 10.4 10.3 D609, D 1730, D1731. D 1732, D 2092.02201 D1640 D 4062, D 2353 D 3793. D 2354 D 3928 D823 D1212 IT fl.t.1 11.1.2 11.1.3 11.1.4 11.2 11.3 D 1739.02616 0 2244 and D 3134 D1535 D 2244 D523 0344,02605 12 12.1 12.2 12.3 12.4 12.4.1 12.4.2 12.4.3 12.4.4 ' 12.4.5 12.4.6 12.4.7 12.4.8 12.4.9 12.5 12.6 12.6 12.8.1 12.8.2 12.8.3 12.8.4 12.8.6 12.8.6 12.8.7 12.8.B 12.8.9 12.7 12.9 12.10 12.4.10 12.11 D 658, D 968. D4060 D 2197, D 3359 D 522, D 1737. D3281 D714 D 859 D 660 D 661 D 662 0 772 . D 610, D 2933 0 822.0 3361.04587 D1654 D 1474 D 2794, D 3170 0 870 D1735 . 02247 D1653 B117,B287 D 2246 02803 D4585 02246 D 1308, 0 1540, D 3023 D2454. D 2091 D 1848 D 1186, D 1400 13 13.2 13.3 13.3 13.4 13.6 0 2369 D 2697 0 2369 D 2371 D 3168 Federal Test Method S 3011.1 ... 2131.1.4331.1 832 i. ft" m .a .1 J-v, DUP050298014 # D 4712 irdaiice with Test Method D 562. '.8 pH--The pH of a water-reducible coating depends on type of vehicle used and the general formulation. It may from about 4 to 10. A change in pH during storage may cate poor stability or a change in properties of a reducible coaling. Determine pH in accordance with Method E 70. jj.9 Freeze-Thaw Resistance--Water-reducible coatings "|iy be subjected to freezing conditions during shipping and ! rage. Suitably stabilized paints will resist several cycles of ng and thawing without showing deleterious changes, referenced method covers the determination of the it to which water-reducible coatings retain their original itency and freedom from lumps when subjected to ng and subsequent thawing. Determine freeze-thaw nee in accordance with.Test Method D 2243. 10 Package Stability--Since liquid coatings cannot nor- be used immediately after manufacture, they must in stable in the package for some time. The referenced method covers the change in consistency and ip certain ated properties that may take place in packaged waterlucibfe coatings when stored at a temperature above room imperature. Determine package stability in accordance with test Method D 1849, at a temperature and, for a period'of le agreed upon by the purchaser and the seller. Nyz' --Although there is no ASTM or Federal test method for ifermining gassing during normal storage, special containers may he l|essary to vent any spontaneous pressure biiildup. 9.11 Microorganism Resistance--Microorganisms in waifrreducible coatings can cause gassing, putrefaction or fomentation odors, and loss of vicosity. Determine if the Tpid coating contains living bacteria and if it is resistant to Sack by bacteria in, accordance with Test Method D2574. 9.12 Surface Tension--Although there is no ASTM or tederal test method for determining surface tension ofliquid Tarings, this is an important property of a water-reducible to or coating. If surface tension is top high, poor pigment id substrate wetting may occur, leading tq cratering, low loss, or other surface defects. The most common methods | measuring the surface tensions of coatings probably are B ring pull method and drop weight method.. For a ^apprehensive discussion of these and other aspects of Surface tension, see Paint Flow and Pigment Dispersion.`6 9.13 Flash Point--Nearly all water-borne coatings, ace capable of sustaining combustion, but many do. contain volatile solvents whose vapors can ignite if near open flame, tecause they do give flash points, water-borne coatings must tested for flash point temperature to conform with many government regulations concerning transportation, labeling, packaging, etc. Determine flash point in accordance with ,;{est Methods D 56, D 93 or D 3278. }>l9.14. Conductivity--Conductivity, is an important factor It the application of some water-borne coatings. Test 'Methods available for determining conductivity are D 1125 ^"'specifically Methods A and B) and D 4399. 10. Application and Film Formation . ?: 10.1 Panel Preparation--Select a substrate as agreed upon P* /1 16 Pation, T,, Paint Flow and Pigment Dispersion, 2nd Ed., Wiley-Inlerscience, Jew York, 1979, pp. 205-246. by the producer and the user. Prepare panels for testing the coating in accordance with Test Methods D 609, D 1730, DI731, D 1732, D2201, or D2092. The preparation of plastics for paint testing is covered in Practice D 3002. 10.2 Application Properties--Determine the ease with which the liquid coating can be applied to various surfaces with brush, spray, or other application equipment. Applica tion properties are generally compared to a standard, or described by requirements in a product specification. Appli cation properties are related to such characteristics as kine matic viscosity, non-Newtonian rheology, surface tension, shear sensitivity, micelle stability, electrical resistivity, ero sion abrasiveness, conductivity, heat capacity, and corrosive ness. 10.2.1 Sprayed Film Application--Liquid coatings can be applied by spray. Determine the spray application properties in accordance with Method 2131.1 of Federal Test Method Standard No. 141. The rnethod can be modified tq include application by airless spray equipment. 10.2.2 Drying Properties---The drying time of water-re ducible coatings is important in determining when, the applied coatings can be handled or packed. Also, inadequate drying of the film may result in'poor filth and poor appearance and, if used on an exterior surface, rain, dew, or snow may cause a nonuniform appearance. Determine drying time in accordance with Test Method D 1640, or as agreed upon by producer of user. 10.3 Leveling Properties--Leveling is an important factor When uniform surfaces are to be produced, as it affects hiding and appearance. The referenced methods cover the labora tory determination of the relative leveling characteristics of liquid coatifigs. Determine the leveling Characteristics in accordance with Test Method D 4062. Measure wet film thickness in accordance with Test Method D 1212. 10.4 Producing Films of Uniform Thickness--The fol lowing test method covers thepreparation ofvarious films of uniform thickness essential in conducting tests. Prepare films in accordance with Test Methods D 823. 10.5 Low Temperature Coalescence of Paints--A test method to determine how well the latex particles to coating will fuse together or coalesce to form a continous .film at low temperature is described in Test. Method D:3793. A test for the minimum film formation temperature is described in Test Method D 2354. 10.6 Touch-Up--For many coating,systems it is impor tant to be able to repair damage sustained during production, delivery, or after delivery. A - coating can be tested by applying it with a small nylon bristle brush or air brush to a small section of a panel previously coated with it. When the touch-up area has dried, it is examined to see if it differs significantly from the initial coating. Determine the ability to touch up the coating in accordance with Test Method D 3928. Test the adhesion of the original and touch-up areas in accordance with Test Methods D 3359 or other agreedupon test method. 11. Appearance of Dry Film 11.1 Color--The color of a water-reducible coating may be specified independently or as the color-difference with respect to another color that is usually the standard. Visual and instrumental methods are both applicable. An opaque 833 f l y0 1 f r 5 S \ 3 3 t 3 1 1 t! DUP050298015 D 4712 film is preferred that may be prepared by making one or more applications of water-reducible coating onto a black and white substrate until the substrate is completely ob scured. Each application should be performed in a normal manner with respect to application method, drying, and film thickness. 11.1.1 Color Differences by Visual Evaluation--Visual comparison of color is fast and often acceptable although numerical values are not obtained. The referenced standard covers the spectral, photometric, and geometric characteris tics of light source, illuminating and viewing conditions, size of specimens, and general procedures to be used in the visual evaluation of color differences of opaque materials. Deter mine color difference by visual evaluation in accordance with Practice D 1729 or Test Method D 2616. 11.1.2 Coldr Differences of Opaque Material by Instru mental Evaluation--Color difference between a product and the standard can be measured by an instrument Generally, the tolerance is agreed upon by the purchaser and the seller and may also be required if a product specification is involved. Color instruments provide numerical values that can be subsequently compared to later measurements. The referenced method covers the instrumental determination of small color differences observable in daylight illumination between nonfluorescent, nonmetameric, opaque surfaces such as coated specimens. If metamerism is suspected, visual evaluation (10,1.1) should be used to verify the results. Make instrumental measurement of color difference in accordance with Method D 2244, Tolerances are discussed in Recom mended Practice D 3134. 11.1.3 Color Description by Visual Evaluation--In some cases it is necessary to specify or identify a color instead of a color difference from some standard. Various color atlases are available, the most common being the Munsell System. Describe or identify the Mtfnsell color in accordance with Method D 1535. 11.1.4 Color Description by Instrumental Evaluation-- Instrumental measurements involve the determination of CIE tristimulus values, X, Y, and Z, from which other color coordinates such as L*. a*, b*, or L, a, b values may be calculated or obtained directly with some instruments. Describe or identify in accordance with Method D 2244. 11.2 Gloss--Water-reducible coatings vary in gloss and the end use determines whether the gloss should be high, semi-gloss, eggshell, or flat. Determine the gloss in accord ance with Test Method D 523 using 20, 60, or 85geometry as appropriate. 11.3 Hiding Power (Dry Opacity)--Hiding power is the measure of the ability of a paint to hide the substrate. It is, however, dependent upon uniform film thickness which is influenced by flow and leveling. Test Method D 344 is a practical test in which paint is applied with a brush, film thickness is approximately measured, and opacity is evalu ated visually as compared to a standard paint. Results are affected by flow and leveling application properties of the paint. Test Method D2805 is considered to be a more precise and accurate test that does not need a material paint standard. Paint is applied with an applicator bar to minimize the effects of flow and leveling, film thickness is rigorously measured, and opacity is instrumentally evaluated. Deter mine hiding power in accordance with Test Methods D 344 or D 2805. 12. Properties of Dry Film 12.1 Abrasion Resistance--Abrasion resistance is a mea- sure of the ability of a dried coating to withstand wear and' marring from objects rolled or pulled across the surface Determine abrasion resistance in accordance with Test Method D 658, D 968, or D 4060 (see methods to determine the applicability for interlaboratory use). 12.2 Adhesion--Adhesion is the property of the coating ; that resists removal from the substrate when scraped. Test Methods D 2197 covers the use of a scrape adhesion tester and a parallel groove adhesion tester. In Test Methods D 3359 cuts are made in the film and pressure-sensitive taj\ applied and removed. Determine adhesion in accordance with Test Methods D 2197 or D 3359. 12.3 Elongation--Elongation is a measure of the flexi bility of coating films. Determine elongation in accordance with Test Methods D 522, D 1737, or D328I. 12.4 Exterior Exposure--If the paint is intended tor exterior exposure, tests may be run in accordance with, Method D 1014, and Standard D 1150 and evaluated by ibg following methods; 12.4.1 Blistering--Determine the degree of blistering ufj$ accordance with Test Method D 714. 12.4.2 Chalking--Determine the degree of chalkingj 1 accordance with Method D 659. 12.4.3 Checking--Determine the degree of checking in accordance with Test Method D 660. 12.4.4 Cracking--Determine the degree of cracking in accordance with Test Method D 661. 12.4.5 Erosion--Determine the degree of erosion'in ac*- cordance with Test Method D 662. 12.4.6 Flaking--Determine the degree of flaking in ac cordance with Test Method D 772. 12.4.7 Rusting--Determine the degree of rusting in ac cordance with Test Methods D 610 or D 2933. 12.4.8 Accelerated Weathering--Determine the resistance to accelerated weathering in accordance with Test Method'-' D 822, D 3361, or D 4587. 12.4.9 Corrosive Environment--Determine the resistance to corrosive environment in accordance with Test Method D 1654. 12.4.10 Reporting of Results--The reporting of results can often be helped by reference to the classifications prescribed in Classification D 1848. 12.5 Hardness--Hardness is a measure of the ability of a dried coating to resist indentation. Determine hardness in accordance with Test Method D 1474. 12.6 Impact Resistance--An important property of water-reducible Coating is its ability to withstand a striking blow or impingement. Determine the impact resistance m .. accordance with Test Methods D 2794 or D 3170. ,, 12.7 Resistance to Chemicals--An important property of a water-reducible coating is its ability to resist spotting, softening,, or removal when subjected to household chemi cals or strong cleaners. Determine resistance to chemicals in ; accordance with Test Methods D 1308 or D 1540 or Practice D 3023. 12.8 Resistance to Various Physical Forms of Water-- 834 DUP050298016 "**'"***-"............... . 4712 The ability of a dried coating to resist water in many different forms is an especially important property of waterreducible coatings. 12.8.1 Water Immersion--Determine the resistance to water absorption in accordance with Practice D 870. 12.8.2 Water Fog--Determine the resistance to water fog in accordance with Practice D 1735. 12.8.3 Humidity Resistance--Determine the resistance to 100 % relative humidity in accordance with Practice D 2247. 12.8.4 Moisture Vapor Permeability--Determine the re sistance to moisture vapor transmission in accordance with Test Method D 1653. 12.8.5 Salt Spray--Determine the resistance to salt spray (fog) in accordance with Methods B 117 or B 287. 12.8.6 Humidity-Thermal Cycling--Determine the resist ance to humidity-thermal cycling in accordance with Test Method D 2246. 12.8.7 Filiform Corrosion--Determine the resistance to filiform corrosion in accordance with Test Method D 2803. 12.8.8 Condensation--Determine the resistance to con densed water such as dew in accordance with Practice D 4585. 12.8.9 Detergent Resistance--Determine the resistance to detergent solution in accordance with Practice D 2248. 12.9 Overbaking--The ability of a coating to withstand a baking temperature moderately higher than initial bake or for a longer period oftime is an important property. Measure the resistance to overbaking by Practice D 2454. 12.10 Print Resistance--Print resistance is the ability of a dried coating to withstand pressure from a textured surface without any noticeable marking on the coating. Measure print resistance in accordance with Test Method D 2091. 12.11 Dry Film Thickness--There are several methods currently being used for determining dry film thickness. Depending on the substrates being used, the following test methods should be considered: D 1005, D 1186, D 1400, and D 2691. 13, Analysis of Paint 13.1 Chemical Analysis--If a specification requires cer tain raw materials or certain components in a given amount, then chemical analysis is required. Chemical analysis deter- mines whether the specified components are present, and if they are, in what amounts. It does not necessarily establish quality, which can also be greatly affected by manufacturing techniques. Most ASTM analytical methods, such as Method D215, apply to solvent-type coatings. However, some of these can be adapted for analysis of water-reducible coatings. 13.2 Volatile Content--The percent of volatile matter indicates the water and organic solvent released from the film as it dries. This quantity subtracted from 100 % gives the nonvolatile content. Determine the volatile content in accordance with Test Method D 2369. 13.3 Nonvolatile Content--The percent of nonvolatile matter indicates the amount of material present that can be converted to the desired film. Determine the weight percent of nonvolatile in accordance with Test Method D2369. Determine the volume percent of nonvolatile in accordance with Test Method D 2697. 13.4 Pigment Content--Although the referenced method describes the procedure for quantitative separation of the vehicle from the pigment in solvent-reducible coatings, it can be adapted for water-reducible coatings to determine the weight percent pigment in the paint. Determine the pigment content'in accordance with Test Method D 2371. 13.5 Pigment Analysis--The analysis of pigment may be required ifthe product is covered by a specification, or if it is agreed upon between the producer and the user. Analyze the pigment in accordance with methods appropriate for the constituents present or specified. 13.6 Identification of Vehicle Solids--The suggested method covers the qualitative characterization or identifica tion of separated paint vehicle solids by infrared spectros copy. It is useful in detecting uniformity, batch to batch, and the presence of adulterants. Characterize vehicle solids in accordance with Practice D 3168. 14. Keywords 14.1 alkyds; appearance of materials; application proper ties; brush application; color; curtain coat; dip application; electrostatic spray; emulsion vehicles; exterior exposure; fancoat; film formation rates; fiowcoat; instrumental evalua tion; opaque film; paints and related coatings; paints, waterbase; roller coat; spray method; visual examination; waterreducible coatings. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination oi the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or v/ithdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouid mate your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 835 DUP050298017 (JjjjM Designation: D 4713 - 87f1 Standard Test Methods for Nonvolatile Content of Printing Inks, Resin Solutions, and Vehicles1 This standard is issued under the fixed designation D47I3; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year ofiast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or rcapprovai. N{|' --Paragraphs 3.2 and 11.1,2 were editorially corrected in May 1988. 1. Scope 1.1 These test methods cover the determination of weight content of nonvolatile matter in two types of printing inks. 1.2 Test Method A is applicable to heatset-type printing inks and resin solutions; solvents in such systems typically have initial boiling points in the range from 240 to 275C (470 to 535"F) and vapor pressures less than 0.2 mm Hg. 1.3 Test Method B is applicable to liquid-type printing inks and vehicles based on aqueous or organic solvents that evaporate readily at ordinary room temperatures. 1.4 This standard may involve hazardous materials, oper ations, and equipment. .This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. N}~' . 1--Test Method A (for heatset systems) specifies a specimen film thickness that is much thinner than those produced by related test methods; one exception is Test Method B in Test Method D 1259, which is recommended as a referee test. N' 2--Test Method B (for liquid ink systems) is similar to Test Method D 2369 except that a solvent is not required for spreading the test specimen. 2. Referenced Documents 2.1 ASTM Standards: D 1259 Test Methods for Nonvolatile Content of Resin Solutions21 D2369 Test Method for Volatile Content of Coatings3 E 1 Specification for ASTM Thermometers4 E 145 Specification for Gravity-Convection and Forced- Ventilation Ovens5 E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method6 3. Summary of Test Methods 3. i Test Method A--Heatset Systems. A 0.15-g specimen is mechanically spread in a 57-mm weighing dish to a nominal thickness of 80 10 g/m2 and heated in a forced ventilation oven at 110C for 3 h. 3.2 Test Method B--Liquid Ink Systems. A 0.5-g spec imen is dispensed into a 57-mm weighing dish by means ofa disposable syringe, mechanically spread out, and heated in an oven at 110'C for 1 h. 4. Significance and Use 4.1 Nonvolatile content of printing inks is useful for specification acceptance between the supplier and the pur chaser.. 4.2 In order to obtain accurate results for heatset systems within the specified 3-h heating time, the specimen film thickness must be less than . 100 g/m2, and the oven must; ' have forced ventilation. Thickness of the specimen film is less critical for liquid ink systems. 5. Apparatus 5.1 Balance, accurate to 1 mg. 5.2 Oven, forced-ventilation type conforming to Type IIB in Specification E 145 and maintained at 110 2C. 5.3 Thermometer; bulb-type, capable of reading 110. vfl 2C, such as Thermometer 88C prescribed in Specification E 1. 5.4 Weighing Dish, such as an aluminum foil dish 57 mnt! wide, the lid of a 1-lb ink can 94 mm wide, or other? flat-bottomed container. The bottom of the container nuisfj not have a trough or depression into which the test material! might collect. 5.5 Spatula, or small ink knife. 5.6 Spreading Device, one per weighing dish, of heatiif stable material, such as a glass stirring rod or thick L-shaped wire. 5.7 Forceps, j|| 5.8 Desiccator, 5.9 Syringe7 (for liquid ink systems only), single-use 2 to, 5-mL capacity without needle, or other weighing device1 listed in the Apparatus section of Test Method D 1259. 6. Reagents 6.1 Toluene, technical grade. 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coalings and Materials and are the direct responsibility of Subcommittee DO 1.56 on Printing Inks. Current edition approved June 26, 1987. Published August 1987. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards. Vols 05.03 and ) 4.03. 5 Annual Book ofASTM Standards, Vol 14.02. b Annual Book ofASTM Standards, Vols 06.03, 08.03, and 14,02. 7. Preparations of Equipment and Sample 7.1 Check the levelness of shelving in the oven; adjust, if necessary. Lay the thermometer on shelf with the bulb at the place where the samples will be placed. Adjust oven controls 3 "| 7 Available from any scientific supply house. 836 DUP050298018 0 4713 Until thermometer reads 110 2C. If air flow is adjustable, : control dampers at 50 %. 7.2 Wear disposable gloves prior to handling weighing spreading device, or syringe in order to minimize pntamination by moisture from hands. :' 7.3 Measure diameter of bottom of weighing dish in liimetres. For example, a catalogue listing of 57 mm refers the top diameter, whereas the bottom diameter may be 50 mm. The bottom diameter must be used in the illations of weight per unit area in 9.3. Mark weighing dishes with a suitable notation. Rinse i toluene and heat in oven at 110C for '/: h. Thoroughly mix ink in container to ensure that the is uniform. Close can after removing specimen. I when finished. Procedure 8.1 Test Method A--Heatset Systems: .1.1 For each specimen, tare to the nearest milligram two ghing dishes each with a spreading device. Retain .ding device throughout the test. `18.1.2 Transfer a representative portion of the sample to tip of a spatula and dab about 0.15 0.02 g around the im of each 57-mm dish, or 0.43 0.02 g ifa 94-mm can used. Quickly reweigh and calculate the weight per unit in accordance with 9.3. If in excess of 100 g/m2, discard weigh out a new specimen. 8.1.3 With spreader, smooth out the specimen into a nably uniform film covering the entire bottom of the High viscosity inks may require a few drops of a e solvent to aid in spreading out the film. 4 Place the dishes in the forced draft oven at 110C for Remove dishes from oven, cool in desiccator, and h.2 Test Method B--Liquid Ink Systems: !2.'l Tare weighing dishes as in 8.1.1. Transfer 2 to 4 mL fepresentative sample to syringe and weigh. Dispense a 0.5 "\1 g specimen from the syringe to a 57-mm dish, or 1.5 to a 94-mm can lid. Immediately spread out as in 8.1.2. i syringe. !.2 Repeat 8.2.1 with second dish. 2.3 Place dishes in forced draft oven at 110C for I h. ove dishes from oven, cool in desiccator, and reweigh. Calculation . 1 Calculate content of nonvolatile matter as follows: NVM, % = (W/S) x 100 specimen weight after heating, g. initial specimen weight, g. f.2 Optioned: The percent of volatile matter may be eulated by difference as follows: VM, % = 100 - NVM %. 9.3 Calculate initial weight/area of each specimen: W/A = 1 000 000 S/3.14 R2, g/m2 where: W = weight, A - area, and R = radius of dish bottom, mm = diameter/2. N' 3--For a dish with a 50-mra bottom diameter, weight/area = SIDS'. For a can lid with a 94-mm bottom diameter, w'eight/arca = 1450 S. 10. Report 10.1 Report NVM to the nearest 0.1 % as the mean of replicate determinations. 10.2 Optional: Report VM to the nearest 0.1 %. 10.3 Report the mean weight per unit area of the initial specimens to the nearest gram per square metre. 11. Precision and Bias 11.1 Fredsion:. 11.1.1 Test Method A--Heatset Systems. An interlabora tory8 study was conducted in which one operator in each of five laboratories tested in duplicate on each of two days four heatset printing inks, of which two were low NVM (about 50 %) and two were high NVM (about 60 %). The roundrobin data were analyzed according to Practice E 691. There were no outliers. The within-laboratory pooled standard deviation was found to be 0.44 % absolute at 12 degrees of freedom, and the between-laboratories pooled standard devi ation was 2.0 % absolute at 16 degrees of freedom. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 11 A.].{.Repeatability--Two results, each the mean of two runs obtained by one operator, should be considered suspect if they differ by more than 1.2 % absolute. 11.1.1.2 Reproducibility--Two results, each the mean of two runs obtained by operators in different laboratories, should be considered suspect if they differ by more than 5.7 % absolute. 11.1.2 Test Method B--Liquid Ink Systems. See Precision section of Test Method D 2369. 11.2 Bias--In the interlaboratory study of heatset inks described in 11.1, the mean values for NVM agreed with the calculated values within 1 % absolute. 12. Indexing Terms 12.1 These test methods are indexed under the following terms: Heatset-type printing inks, ink, nonvolatile matter content, ovens, printing inks, resin solutions, solvents, and vehicles. 8 Supporting data are available from ASTM Headquarters, 1916 Race $u Philadelphia, PA L9103. Request RR D01 - 1053. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised th8t determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revisedeither reapproved or withdrawn. Your comments are invited elther for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. 1916 Race St.. Philadelphia, PA 1310;3 837 DU P 0502 98019 Designation: D 4752 - 87 Standard Test Method for Measuring MEK Resistance of Ethyl Silicate (inorganic) Zinc-Rich Primers by Solvent Rub1 This standard is issued under the fixed desisnation D 4752; the number immediately Mowing the designation indicates the vear of onginai adoption or, in the case of revision, the year odast revision. A number in parentheses indicates the year often reaonroval A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method describes a solvent rub technique for assessing the MEK. resistance of ethyl silicate (inorganic) zinc-rich primers. The MEK resistance of some two-com ponent ethyl silicate zinc-rich primers has been shown to correlate well with the cure of the primer as determined by diffuse reflectance infrared spectroscopy.12 The technique can be used in the laboratory, field, or in the fabricating shop. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 6. 2. Referenced Documents 2.1 ASTM Standards: D740 Specification for Methyl Ethyl Ketone3 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base4 3. Description of Term Specific to This Standard 3.1 double rub--a back-and-forth motion over the test area of approximately 2 in. (50 mm). 4. Significance and Use 4.1 Ethyl silicate zinc-rich primers cure by the reaction of the vehicle with moisture thereby providing a binder. As relative humidity and temperature vary during the day, so does the rate of cure. A certain minimum degree of cure is necessary prior to topcoating. It has been shown that the degree of cure of ethyl silicate zinc-rich primers can be measured by the chemical changes occurring using diffuse reflectance infrared spectroscopy.2 This solvent rub test has been shown to correlate well with the infrared spectroscopic results of two-component ethyl silicate inorganic zinc sys tems. 1 This lest method is under thejurisdiction of ASTM Committee D-l on Paint and Related Coatings and Material and is the direct responsibility of Subcom mittee DO 1.46 on Industrial Protective Coatings. Current edition approved Nov. 27, 1987. Published January 1988. 2 Starr, T. L,, Henton, L. E., Lewis, W. S., and Rideout, F. A.f "Improved Field Reliability of High Performance Coating Systems: Phase II--Develop Procedures and Criteria in Critical Performance Areas," available from Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, PA 15213. 3 Annual Book ofASTM Standards, Vcl 06.03. * Annual Book ofASTM Standards, Vol 06.01. 4.2 The cure rating required for the application of specific topcoats must be agreed upon before the test method is used. 5. Reagents and Materials 5.1 Methyl Ethyl Ketone (MEK), in accordance with :j Specification D 740. 5.2 Cotton Cheesecloth. j 5.3 Squeeze Bottle. I 6. Precautions i* 6.1 Methyl ethyl ketone is a flammable liquid. Its vapors | form explosive mixtures in air. Repeated or prolonged)! contact can cause drying of the skin. Consult supplier s g Material Safety Data Sheet(s) for specific hazard inform firm 7. Procedure 7.1 Select areas on the primer surface at least 2 in. (50 , mm) long on which the tests will be run. Measure the dry film thickness of the primer in the selected areas in accord-,, 1 ance with Test Methods D 1186. ! 7.2 Clean the surface first with fresh water to remow j loose material. ; 7.3 Immediately fold the cheesecloth into a pad cor- j taining four thicknesses of the cloth. Saturate the cloth ti a j dripping wet condition with the methyl ethyl ketone. j 7.4 Rub the test area with the saturated cloth, exertr . 5 moderate pressure with the thumb, using a 2-in. (50-mm) j long stroke that encompasses the test area. | 7.5 Continue rubbing the surface with the MEK saturated g pad, wetting the pad as necessary without lifting it firom t,rc | surface, until either the metal substrate is exposed or 50 J double rubs have been completed. Record the number of rubs when the substrate is exposed. 7.6 Select an adjacent area to be used as a control. Repeat j 7.1 through 7.5, except use a dry cheesecloth to establish the. effect of burnishing without the influence of MEK. |j TABLE 1 Scale for Resistance Rating Resistance Rating ' ~~ Description No effect on surface; no zinc on cloth after 50 double rubi Burnished appearance in rubbed area; slight amount of on cloth after 50 double rubs Some marring and apparent depression of the film after 63 double rubs Heavy marring; obvious depression in the film after 50 dotb'e rubs Heavy depression in the film but no actual penetration to the. substrate after 50 double rubs Penetration to Ihe substrate in 50 double rubs or less___ ^ 838 DUP050298020 ffi D 4752 |.7 Inspect the test areas and the cheesecloths. Rate the (jits in accordance with Table 1. ifepot* J|1 Report the following information: ||1,1 Dry film thickness of the primer. jpj .2 Elapsed time between the application of the primer ||the running of the tests. ||i.3 Number of tests conducted. Resulting ratings. 111.5 In the case of a zero rating, number of double rubs lujred to expose the substrate. 1 6 Field and Fabricating Shop Tests--Identification of the area or piece tested. 9. Precision and Bias 9.1 Since no standard for measuring the MEK resistance of ethyl silicate zinc-rich primers has been developed prior to this test method, precision and bias statements will be developed in round-robin testing. 10. Indexing Terms 10.1 This test method is indexed under the following terms: curing characteristics, double rub method, drying or curing, ethyl silicate (inorganic) primer, methyl ethyl ketone, MEK (methyl ethyl ketone) resistance, primer, solvent rub method, visual examination, and zinc-rich primer. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of thls standard are expressly advised that determination' of the validity 0/ any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must berevlewed every five years and if notrevised, either reapprovad or'WlthdraWn. Yourcomments are Invited either forrevision of thfs'standard orforadditional standards and should be addressed to ASTM Headquarters.-Your comments wilt receive carelul consideration at a meeting of the responsible technical committee, which you may attend, if you feafthatyour comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103, ,, . ------------------------- 839 DUP050298021 Designation: D 4764 - 88 Standard Test Method for Determination by X-ray Fluorescence Spectroscopy of Titanium Dioxide Content in Paint1 This standard is issued under the fixed designation D 4764; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year ofiast revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of titanium dioxide content in liquid paint. This test method is appli cable to both water-reducible and-solvent-reducible paints. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility pf'tM .user of'fhis standard to istablish appropriate safety and 'health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7. 2. Referenced Documents 2.1 ASTM Standards: D476 Specification for Titanium Dioxide Pigments12 D 1 i93 Specifications for Reagent Water3 D1394 Test Methods for Chemical Analysis of White Titanium Pigments2 D2369 Test Method for Volatile Content of Coatings4 D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings4 D3980 Practice for Interlaboratory Testing of Paint and Related Materials4 D 4563 Test Method for Determination by Atomic Ab sorption Spectroscopy of Titanium Dioxide Content of Pigments Recovered from Whole Paint4 E 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial Chemicals5 3. Summary of Method 3.1 Paint containing a known amount of titanium dioxide is used as the reference standard. A solution of tetraethylammonium bromide in 2-ethoxyethanoI is added to the standard paint and to each paint being analyzed. Drawdown films ofthe standard and test paint are made on thin plastic sheets. The intensities of key X-ray fluorescence peaks of titanium and bromine are measured. The titanium dioxide content is determined by comparing the ratio of the intensi ties of titanium and bromine peaks in the test paint and the standard. Differences in the nonvolatile content of the paints 1 This test method is under thejurisdiction of ASTM Committee DOI on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Feb. 26, 1988. Published April 1988. 2 Annual Book ofASTM Standard!, Vol 06.02. 3 Annual Book ofASTM Standards, Vols 06.03 and 11.01. * Annual Book ofASTM Standards, Vol 06.01. 5 Annual Book ofASTM Standards, Vol 15.05. are taken into account in the calculation of results. 4. Significance and Use 4.1 Titanium dioxide pigments are components with hign refractive index that significantly influence the opacity color, durability, and other properties of coatings. This test method for detepnining titanium dioxide content is quicker and easier to use than Test Methods D 1394, a wet chemic il analysis method for pigments. It is conveniently applicable to single samples and to large numbers of samples. Only a single relatively stable reagent used to prepare standards a.iJ paints under test need be stored. Drawdown specimens used as standards, once prepared, can be stored indefinitely air used repeatedly. 5. Apparatus 5.1 X-ray Fluorescence Spectrometer, suitable for mea surement of the baseline corrected intensity of the K lint., of titanium and of bromine. For spectrometers equipp i with a tungsten or chromium target and a lithium fluoride (200) analyzing crystal, these lines are observed at 20 an ks of 86.09 and 29.97, respectively. N' 1--Follow the recommendations of the manufacturer of the , instrument used. Use operating conditions that ensure that the count rate for bromine and titanium are within the linear response range ofthe detector. Although the base operating conditions and count rate may htr different tor different instruments, these differences will not affect tits outcome of the analysis. 5.2 Paint Shaker. 5.3 Film Applicator, to produce a 3-mil (75-pm) wet iih i thickness. 5.4 Plastic Sheet,6 with no interfering X-ray fluorescence peaks and not attacked by paint solvent. 5.5 Perforated Suction Plate, or other flat surface. 5.6 Vials and caps, 20 mL. 6. Reagents 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests, unless otherwise specified. It is intended that all reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Socieis 6 Leneta P-12M0N dull black plastic panels 6l/i by 17 in. by 10 mils (165 hy 432 by 0.25 mm) in size, available from Leneta Co., P.O. Box 576, Ho-Ho-Ku; NI07423, have been found suitable for this purpose. 840 DU P050298022 D 4764 "here such specifications are available.7 Other grades may be sed, provided it is first ascertained that the reagent is of 'iifficiently high purity to permit its use without lessening the ecuracy of the determination. "j 6.2 Purity of Water--Unless otherwise indicated, referjtces to water shall be understood to mean reagent water .at conforms to the requirements of Type II of Specification 1 1193. 6.3 2-ethoxyethanol, purified grade. ; 6.4 Tetraethylammonium Bromide, internal standard sofion--Into a 100-mL volumetric flask weigh .approxi mately 10.80 g of tetraethylammonium bromide (TEAB) to rig. Dissolve the TEAB in 2-ethoxyethanol, fill the flask to \ mark with 2-ethoxyethanol, and mix thoroughly. (TEAB Jpsolved in 2rethoxyethanol can he used as an internal landard for both water-reducible and solvent-reducible "int. However, water may be substituted for 2-ethoxyTiianol, if only water-reducible paint is to be analyzed.) Hazards - 1 ~"'7.1 As exposure to excessive quantifies of x-radiation is 'urious to health, X-ray producing equipment can be angerous to both the operator and persons in the immediate Ijithity Unless safety precautions are strictly observed.' erefore, users should avoid exposing any parts of their dies, not only to the direct beam, but also to secondary or fettered radiation that occurs when an X-ray beam strikes ` passes thrbugh'any material, it is strongly recommended at users check the degree of exposure by film carried on "em o t by the1 use of dosimeters arid that blood counts be %de periodically. Bdfdfe utiliziftg the equipment, all per&s designated or authorized its operate X-ray instniqjenta; `m. or supervise its operation, should have a full undei- nding of its nature and should also become familiar with -tablished safe expdsure factors by a careful study of. the ational Bureau, of Standards' Handbook "X-ray ,Recom- endations of the International Roentgen Ray Committee X-ray Protection,"8 9t1h0e manufacturer's instruction anual, and other standard publications on the subject. uiries should be made of state agencies as to existing quirements. Specimen Preparation 8.1 Thoroughly mix and sample each paint in accordance (h Practice D 3925. Prepare duplicate specimens of the andard paint, which contains a known concentration of "anium dioxide, and each test paint using the following cedure. Into a 20-mL vial weigh approximately 7.00 g of aint to 1 mg. Pipet 2 mL of TEAB internal standard Jution (see 6.4) into the paint and thoroughly mix. 8 2 Place a plastic sheet on the perforated suction plate. the plastic sheet make a 3.0-mil (75-jim) thick drawdown The liquid paint Air dry the drawdown film overnight. Cut 7 "Reagent Chemicals, American Chemical Society Specifications," Am. .arnica! Soc., Washington, DC. For suggestions on the testing of reagents not d by the American Chemical Society, see "Reagent Chemicals and Standards," iiloseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United "s Pharmacopeia." Available from National Bureau of Standards, National Center for Standards, uihersburg, MD 20899. TABLE 1. Instrument Conditions Ti Kff Br K Analyzer crystal Counter Collimator Order Tube KV/mA Time, s Peak, 20, Background, 28, LiF Flow or Sclntiflation Fine First 10/5 20 86.00 85,00 LiF Scintillation Coarse First 60/24 20 29.97 29.00 front the drawdown on the plastic sheet a disk of a size appropriate for the specimen holder of the spectrometer. 8,3 Determine the percent nonvolatile content of each paint at 110C in accordance with Test Method D 2369 if the information is not already available. 9. Procedure 9.1 Turn, on the spectrometer and allow it to stabilize thoroughly before beginning collection of results. With the aid of the manufacturer's literature, select spectrometer settings to permit measurement of the intensity of the Kopeaks of titanium and bromine. For instruments equipped with an X-ray tube with a tungsten or chromium target, the' settings prescribed in Table 1 may be used as guidelines (Note 1). 9.2 Place the disk in the specimen holder in such a way that the coated side of the sheet is turned toward the incident X-rays. Before measuring the specimens, record the back ground spectrum in the ranges of the Ka peaks of titanium and bromine, including at least 10 on each side. Check the spectra for the presence of interfering peaks and select for each peak an angle for background measurement where interference is at a minimum, 9.3 At the selected angles measure the background inten sities and the intensities of the Kcr peaks of titanium and bromine in counts per second (c/s). Determine the net intensity, c/s, of each peak by subtracting the background count from the peak count. 10. Calculation 10.1 Use the values of the standard -paint of known Ti02 content to calculate K,, the reference intensity ratio of titanium relative to bromine in the film, defined as:910 B B+N where: B = TEAB used in making film, g, lb = TEAB used, g, x 100 mL = TEAB used, g, x 50 T = Ti02 in film, g, = paint used, g, x (% Ti02 in dry paint/100) x nonvolatile matter/100, = paint used, g, x % Ti02 in liquid paint/100, 9 Chang, F. H., "A New Approach to Quantitative Multi-element X-ray Fluorescence Analysis," Advances in X-ray Analysis, 19, 1976, p. 81. 10 Chung, F. H., Lentz, A. L, and Scott, R. W., "A Versatile Thin Film Method for Quantitative X-ray Emission Analysis," X-ray Spectrometry. 7(4), 1974, p. 172. 841 DUP050298023 # D 4764 = paint used, g, x weight fraction of Ti02 in liquid paint, N = nonvolatile matter (from paint) in film, g, = paint used, g, x % nonvolatile matter/100, = paint used, g, x % weight fraction of nonvolatile matter, lb = intensity of bromine peak, c/s, and 1, = intensity of titanium peak, c/s. Therefore where: W = paint used, g, and X = weight fraction of TiOj in liquid paint. Calculate the mean of the Kt values obtained from the two disks coated with the standard paint and use in the calcula tion in 10.2. 10.2 Calculate the percent Ti02 in the test paint, P, as follows: _ 2 x B x I, ~K,y.Wxlb where the symbols are defined as in 10.1. 10.3 Sample Calculation; 10.3.1 Reference intensity ratio, K,, Standard paint--12.8 % Ti02 in liquid paint, Standard solution--10.347 g TEAB in 100-mL solution, Film--2 mL of standard solution in 7.25 g of liquid standard paint, and X-ray intensity: Jb = 4396 c/s, I, -- 1804 c/s. K,= 10.347 7.252 x 1 (501(0.128) 1804 = 0.0915 4396 The mean of duplicate analyses is K. - 0.0916. 10.3.2 Ti02 content of test paint, Data: Film--2 mL of standard solution in 7.186 g wet paint, and X-ray intensity: Ib = 4272 c/s, /, = 2569 c/s 10.347 2 2569 7.186 0.0916 4272 18.9 % 11. Precision and Bias 11.1 In an interlaboratory study of this test method, one operator in each of five laboratories analyzed on two days two samples of latex house paint and two samples of solvent-reducible house paint. The mean weight percent titanium dioxide in samples Number 1 through 4 was, respectively, 3.64, 19.1, 7.44, and 15.8 %. The pooled within-laboratory coefficient of variation was 2.39 % with 19: degrees of freedom' and the pooled between-laboratories coefficient of variation 4.47 % with 15 degrees of freedom, after discarding one duplicate value from one laboratory because the range differed significantly from all other dupli cate ranges for paint sample Number 2. Based on these coefficients of variation, the following criteria should be used' forjudging the acceptability ofresults at the 95 % confidence level: 11.1.1 Repeatability--Two results, each the mean of du- ' plicate determinations, obtained by the same operator on different days should be considered suspect if they differ by- more than 7.08 ^ relative. 11.1.2 Reproducibility--Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 13,5 % relative. . The American Society tor Testing and Materials takes no position respecting the, validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of thp validity of any such patent tights, and the risk of Infringement of such rights, are entirely thatr own responsibility. ; This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for addft/pnaf standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. 1916 Pace St., Philadelphia, PA 191Q3. 842 DU P0502 98024 Designation: D 4787 - 88 Standard Practice for Continuity Verification of Liquid or Sheet Linings Applied to Concrete Substrates1 This standard is issued under the fixed designation O 4787; the number immediately following the designation indicates the-year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon () indicates'an editorial change since the last revision or rcappioval. Scope |;i This practice covers procedures that may be used to Sbw the detection of discontinuities iri nonconductive ttings with thicknesses exceeding 20 rails (0,5 mm) applied Igoncrete substrates. 0L2 Discontinuities may include pinholes, internal voids, ilidays, cracks, and conductive inclusions, 1,3 This practice utilizes high-voltage spark testing in Inunction with a continuous conductive membrane. hiYm*:--For further,information on discontinuity testing refer to Nace andard RP0188-88. if.4 ' This standard may involve hazardous materials, 'erations, and equipmenti This standard does not purport to |Iriss all ofthe safetyproblems associated with its use. It is responsibility of the User of this standard to establish ipropriate safety and health^practices and determine the ilapplicability of regulatory limitations 'prior to use. For a S[iecific hazard statement, see Section 6. ( Referenced Documents fc',2.1 ASTM Standards: D149 Test Method for Dielectric Breakdown Voltage and B' ; Dielectric Strength of Solid Electrical Insulating Mate- rials at Commercial .Power Frequencies2 3. >. ri.2 NACE Standards? . 1 RPO188-88 NACE Standard Practice Discontinuity (Holiday) Testing of Protective'Coatings * Terminology : Wf. 1 Description of Terms Specific.to This Standard:, ip. 1.1 discontinuity--a localized' 'fining site that has a ifaectric strength less than a determined test voltage. B3.1.2 conductive underlayment--a continuous layer ap gfeifto the prepared concrete surface prior to.the application "a nonconductive lining layers) that will allow high'voltage ark testing for discontinuities in the lining. jjS.i.3 spark-over--at a certain electrical voltage and disncc from a grounded surface a spark from a high-voltage jlting instrument will jump across the space. 1311.4 high voltage spark tester--a high'voltage electrical 'Itectbr used to locate discontinuities in nonconductive 1 This practice is under the jurisdiction of ASTM Committee D-33 on l 'elective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.04 on Inspection. Current edition approved Sept. 30, 1988. Published November 1988. '2Anrw/il Book ofASTM Standards, Vol 10.01. 3 Available from National Association of Corrosion Engineers, P.O. Box 218340, Houston, TX 77218. linings Applied ter conductive substrate^. 3.1.5 test voltage---that electrical voltage established which will allow a discontinuity at the thickest lining location site to be tested, but which will not damage the lining. The test voltage must always be set well below the dielectric breakdown strength of the lining. This voltage should normally be recommended by the lining manufac turer. The dielectric breakdown voltage strength of a solid can be determined by Test Method D 149. . 4. Summary of Practice 4.1 This practice: allows for high voltage electrical detec tion of discontinuities in new linings applied to concrete substrates through the utilization of a continuous conductive underlayment applied to the prepared concrete surface prior to the application ofthe nonconductive lining layer(s). 5. Significance and Use 5.1 The electrical conductivity of concrete is primarily influenced by the presence of moisture. Other factors which affect the continuity of concrete include the following: .5.1.1 Presence of metal rebars, 5.1.2 Cement content and type, 5.1.3 Aggregate types, 5.1.4 Admixtures, 5.1.5 Porosity,, 5.1.6 Above or below grade elevation, 5.1.7 Indoor or outdoor location, 5.1.8 Temperature and humidity, and 5.1.9 Age of concrete. 5.2 The electrical conductivity of concrete itself may be successfully used for high-voltage continuity testing oflinings applied directly with no specific conductive underlayment installed. However, the voltage required to find a disconti nuity may vary greatly from point to point on. the structure. This variance may reduce the test reliability to an unaccept able level.1 5.3 Although the most common conductive underlayments are liquid primers applied by trowel, roller, or spray, and which contain carbon or graphite fillers, others may take the form of the following: 5.3.1 Sheet-applied graphite veils, 5.3.2 Conductive polymers, 5.3.3 Conductive graphite fibers, 5.3.4 Conductive metallic fibers, and 5.3.5 Conductive metallic, screening. 5.4 Liquid-applied conductive underlayments may be desirable as they can serve to address imperfections in the concrete surface and provide a better base for which to apply the. lining. 843. 'Ll I DUP050298025 # D 4787 5.5 This practice is intended for use with new linings applied to concrete substrates. It may also be applicable for linings previously tested by this practice and subsequently placed in service. However, consideration must be given to potential changes to the electrical properties of the conduc tive and nonconductive layers comprising the system. 5.6 The user may consider this practice when perform ance requirements of the lining in a specified chemical environment requires assurance of a lining free of discontinuities. 5.7 Factors affecting the dielectric properties and test voltage shall be considered. Some factors are the curing time of liquid-applied linings; the possible presence of electrically conductive fillers or solvents, or both; the possible presence of air inclusions or voids; and the compatibility of conduc tive underlayments with the specified lining. 6. Apparatus 6.1 High Voltage Spark Tester--An electrical detector with a voltage rating in excess of 900 V. The detector is to consist of an electrical energy source, an exploring electrode, a ground connection, and ground wire. The detector shall be equipped with a visual or audible indicator, or both. 6.1.1 Electrical Energy Source--Either a-c, d-c, or pul sating d-c type with the appropriate test voltage. 6.1.2 Exploring Electrode--The full length shall be ca pable of maintaining continuous contact with the surface being inspected. 6.1.3 Ground Wire, stranded 14 to 16 gage copper wire. 6.1.4 Visual or Audible Indicators, or both, to signal a closed electrical circuit. Such signals shall be essential for testing the underlayment for electrical conductivity and for exposing discontinuities innhe lining after it has been applied. 7. Hazards 7.1 Solvents retained in the applied conductive underlayment may create an explosive environment as well as produce erroneous results.8 8. Conductive Underlayments 8.1 The conductive underlayment shall not rely on the concrete substrate's electrical properties. 8.2 The specified lining shall be compatible with the specified conductive underlayment. 8.3 Application: 8.3.1 The finished conductive underlayment surface shall be relatively smooth. The conductive underlayment shall be considered part of the lining system and must be installed in accordance with the manufacturer's latest published instruc tions. 8.3.2 Visually verify that the conductive underlayment covers the entire area to be lined. Breaks at expansion joints and construction joints are allowable unless otherwise speci fied. 8.4 Verification of Underlayment Conductivity: 8.4.1 The surface of the applied conductive underlayment shall be clean, dry, free of oil, grease, dirt, or other contaminants and be sufficiently cured in accordance with the manufacturer's latest published instructions at the time the high-voltage spark testing is performed. (Warning--See Section 7.) 8.4.2 Verify the operation of the high-voltage test instru ment in accordance with Section 9. 8.4.3 Adjust the high-voltage test instrument in accord ance with Section 10. 8.4.4 Ground the test instrument to the installed underlayment or other appropriate ground. If electrical isolation across an expansion joint is encountered, the ground wire must be moved to an appropriate ground in the same section being tested. 8.4.5 Place the exploring electrode on a nonconductivi spacer so that an air gap between the surface of tin underlayment and the electrode is equal to the maximum thickness of the lining. 8.4.6 The underlayment is conductive if a spark-over is emitted and the visual or audible indicator, or both, on the test instrument is activated. 8.4.7 Test Sampling. 8.4.7.1 A minimum of four test points shall be used foi the first 100 ft.2 Test points shall be approximately equal!; spaced within the test area. At least one additional test point shall be used for every 500 ft2 thereafter. 8.4.7.2 Test points most distant from the ground connec tion shall be included in the test sampling. 8.4.8 The specified lining shall not be applied until th( conductivity of the underlayment has been verified. 9. Verifying Operation of High-Voltage Spark Tester 9.1 Test electrical source for proper voltage output. 9.2 Follow the equipment manufacturer's operating in structions for verifying the operation of the high voltagetester. 9.3 If the tester fails to signal, it shall be considered defective. 10. Adjustment of High-Voltage Spark Tester for Verifying Conductivity of Underlayment 10.1 Establish the test voltage based on the maximun specified thickness of the nonconductive lining, its dielectric strength, and the lining manufacturer's recommendations. 10.2 Following the equipment manufacturer's instruc tions, set and check the test voltage established in 10.1. 11. Application of the Lining or Coating 11.1 Apply the specified lining in accordance with gov erning specifications. 12. Adjustment of High Voltage Spark Tester for Verifying Conductivity of the Applied Lining 12.1 Select the proper test voltage to provide reliable spark-over to locate a holiday under normal test conditions The voltage selected must jump an air gap equal to the maximum specified dry film thickness of the lining being tested and not arc through the lining at the minimun specified dry film thickness. 12.2 Adjust the tester to the test voltage established in 12.1 as follows: 12.2.1 Connect a high-voltage voltmeter or a spark-gap calibrator between the electrode and the ground wire. 12.2.2 Switch the detector to the ON position. DU P050298026 D 4787 |12.2.3 Perform field checking of the test voltage with the gctrode placed against the surface of the lining since the ploring electrode voltage may be reduced by the slight rrent flow to the lining. P12.2.4 If required, compare measured voltage with the ilected test voltage. Depending on the type of tester, adjust {the selected voltage 5 %. spark testing is performed (Warning--See Section 7). 13.2 Attach the ground wire from the instrument ground terminal to the conductive underlayment or appropriate ground in the same manner as was required in 8.4.4. Make contact with the exploring electrode at a known disconti nuity to verify that the instrument is properly grounded. For each ground location, make contact with a known disconti 12.2.5 Switch the detector to the OFF position. nuity. Conduct this test periodically during the test. 12.2.6 Disconnect the voltmeter or spark-gap calibrator. 13.3 With the exploring electrode in continuous contact with the lining surface, move it over the entire surface of the High Voltage Spark Testing for Verifying Continuity of ; Applied Lining Il3.1 The surface of the applied lining shall be clean, dry, !e of oil, grease, dirt, or other contaminants and be lining at a rate of 1 ft/s (0.3 m/s) maximum in a sweeping motion with overlapping passes to ensure that the entire surface has been subjected to the test. 13.4 Identify discontinuities that require repair with a compatible marker. 13.5 Completely test the lining one time only. Repair all ufflciently cured in accordance with the manufacturer's Eitest published instructions at the time the high-voltage defects found in the lining and retest only those repaired areas. Tha American Society lor Testing and Materials takes no position respecting the validity of anypatent rights asserted In connection with any Item mentioned in this standard, Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is sun/ecf ts revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Your comments are Invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known fo the ASTM Committee on Standards, 191S Race St,, Philadelphia, PA 19103. ? il! fii 845 DUPO 50298 027 Designation: D 4796 - 88 Standard Test Method for Bond Strength of Thermoplastic Traffic Marking Materials1 This standard is issued under the fixed designation D4796; the number immediately following the designation .indicalcs the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (r) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method provides an instrumental means for the determination of thermoplastic traffic marking material bond strengths using cement bricks and steel cubes. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: C 109 Test Method for Compressive Strength of Hydraulic Cement Mortars (Using 2-in. or 50-mm Cube Specimens)12 C881 Specification for Epoxy-Resin-Base Bonding Sys tems for Concrete3 4 D883 Definition of Terms Relating to Plastics'1 E 284 Terminology Relating to Appearance of Materials5 F 412 Terminology Relating to Plastic Piping Systems6 3. Terminology 3.1 Definitions--Definitions are in accordance with Defi nitions D 883, E 284, and F 412, unless otherwise indicated. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 cement brick--a brick formed by mixing cement and fine sand together and allowing to harden. 3.2.2 thermoplastic--traffic marking (same as 3.2.3). 3.2.3 thermoplastic traffic marking--a highly filled 100 % total solids highway marking system that when heated to a molten state can be extruded or sprayed onto a road surface and when cooled forms a solid durable delineator. 4, Summary of Test Method 4.1 The thermoplastic specimen is prepared for this test by first melting a sample to its application temperature under continuous agitation. The specimen is then applied to the specified cement brick by a hot drawdown blade. Two 1 This test method is under the jurisdiction of ASTM Committee D*l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.44 on Traffic Coatings. Current edition approved Oct. 31, 1988. Published December 1988. 2 Annual Hook ofASTM Standards, Voi 04.01. 3 Annual Book ofASTM Standards, Vol 04.02. 4 Annual Bonk ofASTM Standards, Vol 08.01. 3 Annual Book ofASTM Standards, Vol 14.02. 4 Annual Book ofASTM Standards, Vol 08.04. steel cubes are then immediately placed onto the hot thermoplastic line and the excess thermoplastic trimmed away from around the two steel cubes. After the trimmin, s complete, the steel cubes are removed. A heated steel cube is bonded with epoxy to the square of thermoplastic and allowed to cure overnight before determining the bond strength on a Dillon dynamometer or similar device. 5. Significance and Use 5.1 The function of this test method is to provide numer ical instrumental results indicating the cohesive or adhesive or both, bond strength of thermoplastic traffic marking lo i specified cement brick substrate: 5.2 The use of this test method allows the user and manufacturer to control the quality ofthe product and make-, inferences about the performance of the thermoplastic traffic marking product. Results from these tests also provideinformation helpful in researching and developing thermo plastic traffic marking materials. 5.3 Strict adherence to the procedures outlined is neces sary for precision of the test method. Under no conditions should the bond strength be accepted unless there is ecuformance to 9.14. Precise results are obtained only when one steel block is epoxied to the thermoplastic traffic marking on the cement brick. 6. Types of Separation in Bond Strength Tests 6.1 Thermoplastic lo Steel Cube Separation--This type of separation occurs where there is an insufficient bond be tween the thermoplastic and steel cube probably due to1 insufficient coverage of the epoxy adhesive. 6.2 Thermoplastic to Thermoplastic Separation--This type ofseparation is caused by internal cohesive failure of the thermoplastic. This separation is acceptable when it exceeds) the specified bond strength. 6.3 Thermoplastic to Cement Brick Separation--This type of separation is caused by the failure of the bond between the thermoplastic specimen and the cement brick. 6.4 Cement Brick to Cement Brick--This type of sepaution is caused by the internal cohesive failure of the brie. This is due, in most cases, to a bond between the therm plastic and cement brick that exceeds the cohesive strength: of the cement brick. This separation is not acceptable > en the bond strength values are lower than specified. 7. Apparatus 7.1 Agitator Blade, 6 in. (15 cm) long with a `/2-in. (1-cm) steel shaft and a 1% by I in, by '/s-in. (4.5 by 2.5 by 0.3-rm) straight horizontal steel blade. 7.2 Capped Bolts, two, V* in. (16 mm) in size. 846 DUP050298028 5/8 in, NUT < D 4796 600 400N 20D0 ILLD8N00\ , DYNAMOMETER ,2800 1200/ ,24 00 1600/ 20Q<L 5/8 in. FUAT WASHER 5/8 !n.X 2 n . HEX HD. BOLT /'"EPOXY JOINT /"CEMENT BRICK - WELD 5/8 in. NUT TO ' VC6 CHANNEL wt. 8.2 75 inxi 2,7b in, I 7| r-- 6.0 in. | . 1 25 in FIG. 1 Bond Strength Testingj Apparatus 7.3 Cement Bricks, 3'/2 by 2 by 7 `/2-in. (9 by 5 by 19 cm) size with a compressive strength of 3000 to 5000 psi (Note )NE 1--Concrete bricks conforming to Test Method C !09 have used but proved more variable due to migration of a thin veneer of t to the top of the brick making determinations erratic. The t bricks,may be obtained from local block ..plants. The term ment" brick is common for the industry and is used in this test '4thod extensively, |N' 2--The unit should be fitted with a steel frame to hold the 'mem brick for testing. ' 7.4 Dynamometer,7 with a capacity of 6000 lbs in 254b jjijvisions having a pull-rate capability of lA in./min. (Note 2) f.See Figs. 1,2, 3, and 4). Jr 7.5 Draw Down Blade, 2 by I by 4 in. (5 by 2.5 by 10 cm) in size capable of laying down a 125 mil (0.125 in.) wet jhermoplastie film 2 in. wide. \ 1.6 Drill Press, or other apparatus capable of agitating the 'lermoplastic during meltdown to the application tempera.fute at 600 to 800 r/min in the jacketed electric pots. A 7.7 Epoxy Resin and Hardener, Type I or II, Grade 2, i( kiss C in accordance with Specification C 881. ' 7.8 Hot Plate, capable of maintaining 537"C. 7,9 Gravity Convection Oven,1 capable of maintaining TC. .10 Electric Pots, Jacketed, for heating and melting the thermoplastic to 218C. 7.11 Spatulas, for cutting, stirring, and shaping the ther moplastic. i 7.12 Steel Cubes, two, 2 by 2 by 2 in. (5 by 5 ,by 5 cm) in ire threaded in the center of one side for a Vs-in. (16-mm) gapped bolt. considering the physical form of the material. 9. Procedure 9.1 Under continuous agitation melt a specimen of the thermoplastic to be tested to-a temperature of 218"C. If the specimen is a dry powder mix, allow the specimen to-cool to -DRILL & TAP 5/8-18 in. X 3/4 , in. DEEP 0 in. STEEL CUBE ~*"i 1 0 in. 0.625 in. , I f (T Y P) sjl. Sampling Samples may be obtained by an appropriate quar^ei ng or riffle sampling method where deemed necessary I 25i n .--~ll A Dillon Dynamometer available from Weigh-Tranex, 1000 Armstrong ifcnve, P.O. Box 1000, Fairmount, MN 56031, or equivalent, has been found jpuitnblc for this purpose- 847 2.0 in FIG. 3 ' Load Plate (2 Required) DUP050298029 # D 4796 HOLE FIG. 4 Coupling Hitch 193C under continuous agitation and reheat under agitation to 218C. N' 3--Dry powder mixed thermoplastic must be conditioned to ensure a homogeneous melt necessary for consistent results. Premelted block thermoplastic does not require this conditioning. The specimen may be melted on a hot plate set at 537"C or in a jacketed electric pot. Continuous agitation is necessary to prevent scorching and settling. If the specimen is melted in an oven set at 260*C, the specimen must be agitated every 15 min until 218C is reached. 9.2 Heat the draw down blade to 218C. 9.3 Obtain a dry room temperature cement brick that has been brushed or textured on the side to be coated with thermoplastic. 9.4 Heat one 2 by 2 by 2 in. (5 by 5 by 5 cm) steel cube in an oven or on a hot plate to 49I>C for 2 h prior to making the thermoplastic draw down on the cement brick. 9.5 When the thermoplastic specimen is melted to 218C under continuous agitation, remove the agitator blade from the thermoplastic, 9.6 Remove the draw down blade from the hot plate and immediately place it on the cement brick and make the draw down the full length of the brick with the melted thermo plastic on the brushed or rough textured side of the brick. 9.7 Immediately place two room temperature steel cubes on the thermoplastic approximately 1 in. from each end of the brick and trim the plastic from around the two steel cubes before the plastic cools and hardens. 9.8 Remove the steel cubes by hand and allow the thermoplastic to cool for 1 h. 9.9 Prepare the epoxy solution using the proper resin and hardener ratio and mix thoroughly. 9.10 Remove the steel cube heated to 49C from the oven and place a small amount ofepoxy on the heated cube. P[ace' the steel cube on the thermoplastic square and rub to ensure 1 an even coating and good adhesion. To ensure an event coating, remove the steel cube from the thermoplastic square I and visually inspect the square and cube and then replace the J steel cube on the square and rub. Do not allow any excess! expoxy solution to flow from the steel cube and thermoplastic square onto the cement brick. N' 4--Only one steel cube can be epoxied at a lime to the thermoplastic on the brick because the shock of the first pull will cause a premature release of the second thermoplastic square. 9.11 Place a weight such as a cement brick on the steel cube epoxied to the thermoplastic square and allow to cure for a minimum time of 8 h. 9.12 Screw the Vs-in. (15.9-ram) capped bolt into the steel cube epoxied to the thermoplastic and place the brick into : the steel frame mounted onto the dynamometer. 9.13 Set the dynamometer to zero and pull the steel cube at >A in./min. 9.14 Two tests are run on each brick. Separations ,r,volving at least 80 % of the thermoplastic area to the cement4 brick, thermoplastic to thermoplastic, and cement brick to ' cement brick are acceptable for reporting bond strengths. 10. Calculations 10.1 Calculate the bond strength as follows: 10.1.1 Average the readings obtained in 9.13 if the condi-, tions in 9.14 are met. 10.1.2 Divide the average reading obtained by 4. The' result is the bond strength in pounds per square inch. 10.1.3 Ifone ofthe two tests fails then that test is repeated until the conditions of 9.14 are met. 11. Report 11.1 Report the following information: 11.1.1 The type of separation and bond strength, the e batch number, color, and type of thermoplastic. 11.1.2 The determination of the area of separation is subjective. The area not involved in the separation is usualh attached to the steel cube or cement brick. 12. Precision and Bias 12.1 Precision--No general statement of precision can be j made because of lack of sufficient data at this time. 12.2 Bias--No statement of bias can be prepared for 1 test method since there is no absolute method for use as 3 comparative basis. 12.3 Experience dictates that test results with 50 psi are s acceptable. 13. Index Terms 13.1 This test method is indexed under the following terms: thermoplastic--traffic marking; bond strength; <~ment brick. 848 DUP050298030 D 4796 The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, ere entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, oithcrreapproved or withdrawn. Your commmts areinvitedeither forrevision of this standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 1Q103. 849 DUP050298031 Designation: D 4797 - 88 Standard Test Methods for Chemical and Gravimetric Analysis of White and Yellow Thermoplastic Traffic Marking Containing Lead Chromate and Titanium Dioxide1 This standard is issued under the fixed designation D 4797; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 9* 1. Scope 1.1 These test methods cover procedures for the chemical and gravimetric analysis of white and yellow thermoplastic traffic marking containing lead chromate and titanium dioxide pigment. 1.2 The analytical procedures appear in the following order: Percent Binder Percent Glass Beads (Note l) Percent Titanium Dioxide Percent Lead Chromate and Analysis of Chrome Yellow and Chrome Orange Pigments (Nate 2) Sections 10 11 12 13 1.3 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. N' 1--Test for 1.50 glass spheres only. N' 2--This modified analysis of chrome yellow and chrome orange pigments must be used because the heat resistant chrome yellows in the thermoplastic cannot be analyzed by Test Method D 126. 2. Referenced Documents 2.1 ASTM Standards: D126 Test Methods for Chemical Analysis of Yellow, Orange, and Green Pigments Containing Lead Chro mate and Chromium Oxide Green2 D 883 Definitions of Terms Relating to Plastics3 D 1193 Specification for Reagent Water4 5 D 1394 Test Methods for Chemical Analysis of White Titanium Pigments2 F 412 Terminology Relating to Plastic Piping Systems3 3. Terminology 3.1 Definitions--Definitions are in accordance with Defi nitions D 883 and F 412, unless otherwise indicated. 3.2 Descriptions of Terms Specific to This Standard: 1 These test methods are under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Current edition approved Oct. 31, 1988. Published December 1988. 2 Annual Book ofASTM Standards, Vo) 06.02. 3 Annual Book ofASTM Standards, Vols 08.01 and 08.04. 4 Annual Book ofASTM Standards, Vols 06.03 and 11.01. 5 Annual Book ofASTM Standards, Vol 08.04. 3.2.1 ash--the inorganic components of thermoplastic traffic marking including the pigment, glass spheres, and filler. 3.2.2 binder--the organic components of thermoplastic traffic marking that bind the pigments, glass spheres, and filler together as a unit. 3.2.3 filler--the inorganic components of thermoplastic traffic marking not including the pigments or glass spheres. Jf'.': 3.2.4 pigment--titanium dioxide and lead chromate colorants. 3.2.5 thermoplastic--See thermoplastic traffic marking. 3.2.6 thermoplastic traffic marking--a highly filled 100% total solids highway marking system that when heated to a molten state can be extruded or sprayed onto a road surface and when cooled forms a solid durable delineator. 4. Summary of Test Method 4.1 The thermoplastic material is prepared for the de scribed test methods by melting a sample to its application temperature under continuous agitation. The specimen is then poured into round patties on a clean tin plate or baking pan. The patties are then broken into pieces for ignition in a muffle furnace. The percent binder is calculated from the ashed specimen and the various tests for glass spheres, titanium dioxide, and lead chromate pigment are performed on the ashed residue. The tests for pigment type or glass spheres may be run on the same ashed specimen. Specimen selection and preparation are the same for each sample .5 tested. 9 5. Significance and Use 5.1 The function of these test methods is to define the percent of binder, glass, titanium dioxide, and lead chromate present in the composition of the thermoplastic traffic marking as defined by the applicable specification for the manufacture of a specific thermoplastic traffic marking. 6. Apparatus 6. i Balance, analytical, accurate to 0.1 mg. 6.2 Buret, 10 mL, 0.1 -mL divisions. 6.3 Buret, 50 mL, 0.1-mL divisions. 6.4 Crucibles, 30 mL, porcelain. 6.5 Desiccator. 6.6 Erlenmeyerflask, 500 mL. 6.7 Furnace (Muffle), capable of maintaining 1100C. 6.8 Hot plate, capable of maintaining 537C. 6.9 Jones Reductor. V /tern "'listed ^by Jo: ; Slates 850 M DUP050298032  D 4797 6.10 Mortar and Pestle, glazed ceramic or other imperous type. 6.11 Oven, capable of maintaining 260C. 6.12 Sieve, 3 in., 45-^m (No. 325) (metal). ; ' ' 'Reagents 7.1 Purity ofReagents--Reagent grade chemicals shall be ed in all tests. Unless otherwise indicated, it is intended at all reagents shall conform to the specifications of the ommittee on Analytical Reagents of the American ChemIfol Society, where such specifications are available.6 Other fedes may be used, provided it is first ascertained that the eagent is of sufficiently high purity to permit its use without isening the accuracy of the determination. fc7.2 Purity of Water--Unless otherwise indicated, referIpces to water shall be understood to mean reagent water as Refined by Type IV of Specification D 1193. >7.3 Alcohol--Ethyl alcohol 95 %. 1:7.4 Potassium Chloride (K.C1). 1:7.5 Potassium Hydroxide Solution--Dissolve 50 g of potassium hydroxide (KOH) in 100 mL of freshly distilled ater. 1,7.6 Potassium Iodide (KI). p7.7 Potassium Permanganate Solution (KMn04) (0. IN). if .8 Sodium Thiosulfate, Standard Solution (NA2S20> |H20) (0.1 N), t7.9 Starch (Soluble) Indicator Solution--Dissolve 10 g of Sluble starch in 1 L of deionized or distilled water, bf. 10 Hydrochloric Acid Solution (HC1) (1+2). 17.11 Hydrochloric Acid, Concentrated (HC1). Sampling j|8.1 Samples may be obtained by an appropriate quarrig or riffle sampling method where deemed necessary onsidering the physical form of the material. ? Preparation of Specimens jb.l Melt a sample of approximately 10Q0 g of thermolastic traffic marking to 210 to 218C under continuous litation on a hot plate set at 537C or stir every 15 min in |fet>ven set at 260C. fe.2 Flow the sample out on a smooth clean surface and few it to cool to room temperature. Patties l/s in. (3 mm) pbk will facilitate breaking up specimens for the described ||ysis. jj<,3 Break the specimen into small pieces and weigh 10 g p&e nearest 0.1 mg into a 30-mL weighed crucible. 9.4 Cover the crucible and place into a muffle furnace eheatcd to 540C arid ash for 1 h or until no carbonaceous ateriais remain. 3*. 9.5 Remove the crucible with the ashed remains of the j- ^Specimen and place into a desiccator and cool to room ! ^temperature. |pM "Reagent Chemicals, American Chemical Society Specifications," Am. '.Cji'TnjcaJ Soc., Washington, DC. For suggestions on the testing of reagents not j|j|cd by the American Chemical Society, see "Reagent Chemicals and Standards," Jo,eph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the "United ,s Pharmacopeia." 10. Percent Binder 7 10.1 Procedure: 10.1.1 Weigh the crucible and ash (see Section 9) to the nearest 0.1 mg and calculate the percent of organic binder D as follows: D = [1 - (S/H0] x 100 where: S -- ashed weight ofthermoplastic specimen, g, and W = weight of thermoplastic specimen, g. 11 Percent Glass Beads 11.1 Interferences--Acid-insoluble fillers will affect the glass-sphere analysis and must be removed by some physical separation method or accounted for quantitatively, or both. 11.2 Procedure: 11.2.1 Weigh the crucible and ash (see Section 9) to 0.1 mg and calculate the percent ash. 11.2.2 After the ashed material has been weighed, transfer the ash to a mortar and pestle and grind with minimal pressure to reduce the ash to a fine grained consistency without crushing the beads. Carefiilly transfer the ashed contents into a 400-mL beaker. 11.2.3 Add to the ash approximately 150 mL of cold I +2 HC1 and stir occasionally until the effervescence has ceased completely. 11.2.4 Place the beaker on a hot plate preheated to approximately 260C and boil for 20 min under continuous agitation to dissolve all acid-soluble filler pigments. 11.2.5 Remove the beaker from the hot plate,'and while hot, immediately dilute the contents with 150 mL of cold water. Allow the beads to settle. Decant the water carefully so as not to lose ahy glass beads. 11.2.6 Continue diluting with 150-mL aliquots of water and decanting until the water is nearly clear. Then transfer the residue into a weighed 3-in. 45-pm (No. 325) sieve and wash with 500 mL of cold water. 11.2.7 Dry the sides and the bottom of the sieve with a paper towel and dry for 1 h in a gravity oven preheated to 100`C. ' 11.2.8 Place the sieve in a desiccator and cool to room temperature. Weigh the sieve and glass beads to 0.1 mg and calculate the percent beads G as follows: G = (B/W) x 100 where: ' B -- weight of the glass beads, g, and W = weight of thermoplastic specimen, g. 12. Percent Titanium Dioxide 12.1 Procedure: 12.1.1 Weigh the crucible and ash (see Section 9) to 0.1 mg and calculate the percent of ash which is also equal to the percent filler (pigments and beads). 12.1.2 After weighing the above ashed materials, carefully transfer the ash to an agate or similar impervious-type mortar. Grind the ash to a consistent fine powder except for the glass beads. The pulverized ash must be stirred each time specimens are taken to weigh the prescribed amount for the analysis. 12.1.3 Weigh 1 0.1 g of ash for the titanium analysis. 851 DUP050298033 w D 4797 12.1.4 Proceed with the titanium analysis as described in Test Methods D 1394. The Jones Redactor or aluminum reduction method may be used. 12.1.5 At the end of the digestions described in Test Methods D 1394, filter the undigested materials through a' 3-in. 45-p.m (No. 325) sieve with hot water. This will prevent clogging of the Jones Reductor. This step is not necessary if the aluminum reduction method is used. 12.1.6 Calculate the percent of titanium dioxide (TiO,) from the total ash weighed. The result gives the percent of TiO, in the total thermoplastic specimen. 12.1.7 Calculate the percent ash A as follows: A = (S/W)x 100 where: S = weight of ash, g, and W = weight of thermoplastic specimen used, g. 12.1.8 Calculate the percent of total Ti02 in the T based on percent ash: T = 0.08 AMN/CSa where: A = ash (pigment + filler + beads), %, Sa - weight of ash used, g, M = amount, of 0.1 N potassium permanganate (KMn04) solution used, mL, (see. the paragraph on titration with KMn04 solution of the Procedure section of the Jones Reductor Method of Test Methods D 1394), N = normality of KMnCX, used, C = correction factor for Ti02 pigment used (usually 1.0).' This, represents the purity of the pigment if specified, and 0.08 = weight of Ti02 per 1 mL of 1 N KMn04, g. 13. Percent Lead Chromate 13.1 Procedure: . . 13.1.1 Weigh the crucible and ash (see Section 9) to 0.1 mg and calculate the percent of ash. 13.1.2 After weighing the above ashed materials, carefully transfer the ash to an agate or similar impervious type mortar and grind the ash to a consistent fine powder except for the glass beads. The pulverized ash must be stirred when specimens are taken to weigh the prescribed amount for the analysis. 13.1.3, Weigh I 0.1 g of the ash for the lead chromate (PbCr04) analysis. 13.1.4 Analyze the dry ash as follows: 13.1.4.1 Transfer the ashed specimen to a 500-mL Erlentneyer flask. Add 6 mL of the (KOH) solution (see 7.5) and 10 mL of distilled water. Heat until dissolved. Do not allow to dry. To the hot solution add 50 g of KC1. Dilute with water to 200 mL and swirl until dissolved. Add 16 mL of HC1 slowly. Add 10 g of KI and titrate with the standard sodium thiosulfate solution (see 7.7) using the starch solution (see 7.8) as the indicator. Titrate to a green endpoint. N' 3--A 10-mL buret may be used since the titrant required is small for most thermoplastic analysis. 13.1.5 Calculate the percent ash A as follows: A -- (S/W) X 100 ' where: S = weight of gas, g, and . W = weight of the thermoplastic specimen used, g. 13.1.6 Calculate the percent oftotal PbCr04 in the sample (binder + filler) L based on percent ash as follows: L = 0.1077 AMN/CSa where: ash (pigment + filler + beads), %, C correction factor for PbCr04 pigment used (for ex ample, 90 to 100 %, normally 1.0). This represents the purity ofthe pigment if specified; M = amount 'of 0.1 N sodium, thiosulfate solution usee mL, . N = normality of sodium thiosulfate used, and Sa = weight of ash used, g. 14. Precision and Bias 14.1 No general statement of precision can be made because of lack of sufficient data at this time. 14.2 No statement of bias can be prepared for this test method since there is no absolute method for use as a basis for comparison. 15. Index Terms 15.1 This test method is indexed under the following f terms: glass spheres (in traffic paint); lead chromate; tita- * nium dioxide; thermoplastic traffic marking material. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of _thfs standard are express// advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical commlttee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wiii receive careful considaration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, ISIS Race St., Philadelphia, PA 19103. 852 DUP0502 98034 Designation: D 4828) - 91 ate nL '.5) not ute <L ard ion d is Jple exithe sed. kde test asis. 'ing ;ita- Standard Test Method for Practical Washability of Organic Coatings1 This standard is issued under the Fixed designation D 4B28; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. Scope i 1,1 This test method covers the determination of the Native ease of removal of common soli and stains from interior coatings by manual or mechanical washing with a ponge and a liquid or powder cleanser. 1.2 This standard does not purport to address all of the |gfety problems, if any, associated with its use. It is the Isponsibility of the user of this standard to establish appro- date safety and health practices and determine the applica bility of regulatory limitations prior to use. . Referenced Documents *2.1 ASTM Standards: tD 1193 Specification for Reagent Water2 |lD3450 Test Method for.Washability Properties of Interior Architectural Coatings3 pD3924 Specification for Standard Environment for Con- ditioning and Testing Paint, Varnish, Lacquer, and Related Materials3 i Summary of Test Method 3.1 The test material is applied to a plastic panel and Slowed to dry for 7 days or as mutually agreed. Soilants or pains, or both, are applied to the film. The film is washed for to 100 cycles using a sponge and a liquid or powder leanser. After rinsing and drying, the panel is evaluated for jie degree of soil or stain removal, difference in erosion, and ]jy change in gloss/sheen or color between the washed and (washed area. t Significance and Use 14.1 Interior architectural paints are subjected in use to oiling by dirt or other stains. This test method provides a Jjjy to assess relative ease of soil or stain removal from a S|nt film using materials common to households. This test gethod includes a way to evaluate the film for washability Ibperties and changes in appearance. Thus, a formulator #ay evaluate the effects of composition on the washability ibperties of a paint. Users may also compare the ease of soil aoval from difference paints that are tested, preferably at Be same time. This test method is under the jurisdiction of ASTM Committee D-I on Paint Related Coatings and Materials and is the direct responsibility of Subcom mittee D0I.42 on Architectural Finishes. |Current edition approved Oct. 15, 1991. Published December 1991. Originally j&blished as D 4828 - 88. Last previous edition D 4828 - 88. Annual Book ofASTM Standards, Vo! 06.03 and 11.01. Annual Book ofASTM Standards, Vol 06.01. 5. Apparatus 5.1 Sponge and Holder.* . 5.2 Soil and Stain Applicator (see Fig. 1). ; 5.3 Weight, 100 g. , .^ 5.4 Balance, weighing accurately to 0.1 g. 5.5 Doctpr or Bird Film Applicator, having a 7-mil {0.18- mm) clearance by 6-in. (150-mm) film width. 5-6 Glass Plate, .17'h by 6V2 by `A in. (455 by 165 by 6.3 mm). 5.7 Washability Machined 5.8 Black Plastic Panels.6 ' 5.9 Masking Tape. 1 5.10 Straightedge, approximately 17 in. (430 min) in length. 5.11 Cotton'Tipped Swabs. 5.12 Medicine Droppers: 5,13 Suction Plate, for drawdowns. 6. Reagents and.Materials , 6.1 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type IV of Specification D 1193. 6.2 Soil and Staining Medium--Examples found acceptable.for use with this test method include, but are not limited to pencil, crayon, mercurochrome, ball-point pen, waterborne felt-tip markers, lipstick and mineral-oil-bome soilant as outlined in Test Method D 3450. 6.3 Cleaning Media--Examples found acceptable for use with this test method include, but are not limited to, commercial liquid cleansers, laboratory standardized liquid cleaners as outlined in Test Method D 3450, and powder cleansers. Powder cleansers containing chlorine may effect the color of the washed portion of the test panel. 7. Preparation of Apparatus 7.1 Washability Machine--Level the apparatus before use and operate at 37 1 cpm. (A cycle consists of a complete forward and reverse stroke.) 7.2 Sponge and Holder--AAA sufficient weight to the 4 A sponge, 3' by 33A by P/4 in. (75 by 95 by 45 mm). Part No. AG-8! 16, and a metal holder, Part No. AG-8115, available from BYK-Gardner, Inc., 2435 Linden Lane, Silver Spring, MD 20910 or a sponge, Part No. WA 2222, and metal holder, Part No. WA 2220, available from the Paul N. Gardner Co., 316 N. E. First Street, Pompano Beach, Florida 33060-6699 have been found acceptable for this purpose. An equivalent may be used. 5 Washability machine, Model AG-8100, available from BYK-Gardner, Inc. or Model WA 2037D, available from the Paul N. Gardner Co., have been found suitable for this purpose. Other straight-line wash testers may be adapted to meet the requirements of this test method. 6 Leneta P-121-1 ON dull black plastic panels, 17 by 6V2 in. by 10 mils (430 by 165 by 0.25 mm), available from the Leneta Co., P.O. Box 86, Ho-Ho-Kus, N.J. 07423, are suitable for this purpose. An equivalent may be used. 853 DUP0502 98035 A D 4828 prior to 100 cycles, stop and record the number of cycles before proceeding to 8.8. 8.7 Mechanical Method: 8.7.1 Place the sponge and holder at one end of the panel so that its long axis is parallel to the length of the panel (see Fig. 2). Attach to the cable ofthe washability machine. Allow the sponge to travel a maximum of 100 cycles. If all the soils or stains are removed prior to 100 cycles, stop and record the number of cycles before proceeding to 8.8. 8.8 Remove the test panel and evaluate the condition of each soil or stain in the path of the sponge and rate as follows: 0--No change from original intensity (depth) of soil or stain, 3--Slight change from original, but readily visible, 5--Moderate change from original, slightly visible, 7--Large change from original, barely visible, and 10--All soil and stain removed. If a difference exists between a pair of lines, report the lower rating of the pair. When a soil or stain is removed prior to 100 cycles, assign a rating of 10 and note the number of cycles in which each soilant or stain was removed. 8.9 Rinse the panel with running tap water and remove any clinging particles of cleaning medium by gently moving the palm of the hand over the path the sponge followed during the washing cycle. Blot the panel and allow to dry. Rate the washed area relative to the unwashed areas for gloss or color change and erosion as given below: Gloss Change Color Change Erosion N--None I--Increase II--Large increase D--Decrease DD--Large decrease N--None SD--Slightly darker CD--Considerably darker SL--Slightly lighter CL--Considerably lighter N--None S--Slight M--Moderate 9. Report 9.1 Report the following information: 9.1.1 Type of soilant(s), stain(s), washing medium(s) and washing method used and the results obtained in 8.8 and 8.9 9. i .2 Any soils or stains that were removed in less than 100 cycles, and 9.1.3 Any deviation from the recommended procedure. 10. Precision and Bias 10.1 Precision--On the basis of interlaboratory tests in which operators in seven laboratories using the manual washing method, tested four coatings including solvent- and waterborne systems covering a range of pigment volume concentrations, the following criteria should be used for judging the acceptability ofthe results at the 95 % confidence ' level: 10.1.1 Repeatability--Two results obtained by the same operator should be considered suspect if they differ by more than 20 % of their mean rating with the powder cleaner and 40 % with the liquid cleanser. 10.1.2 Reproducibility--Results obtained from the four round robins indicate that the manual method is not suitable ' for between laboratory evaluations. 10.1.3 A precision and bias statement for the mechanical1 method is being developed. 10.1.4 Bias--Bias cannot be determined for this test method. 11. Keywords 11.1 cleansability; soil/dirt resistance; stain resistance; washability; wet abrasion resistance The American Society for Testing anti Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technics! committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either torrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wlil receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feei that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. 1916 Race St., Philadelphia, PA 19103. 856 tfiol DUP050298036 Designation: D 4834 - 88 Standard Test Method for i Detection of Lead in Paint by Direct Aspiration Atomic % Absorption Spectroscopy1 r. This standard is issued under the fixed designation D 4834; the number immediately following the designation indicates the year of * original adoption or, in the case of revision, the year oflast revision. A. number in parentheses indicates the year oflast reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovai. 'gf. Scope 4.1 This test method is intended as a screening test to termine if the solids in a paint contain more than 0.06 % d. The test described can differentiate between 0.05 and 6 %. Paints giving a result greater than 0.05'% should be jgalyzed quantitatively for lead using Test Method D 3335. is test method provides a more definitive and reliable eening test than Test Method D 3618. 1.2 There is no reason to believe that higher levels of lead did not be determined by this test method provided that propriate dilutions and adjustments in specimen size and gent quantities are made. 1.3 This standard may involve hazardous materials; operpns, and equipment. This standard does not purport to Iffejj all ofthe safety problems associated with its use. It is ^responsibility of the user of this standard to establish -ropriate safety and health practices and determine the licability ofregulatory limitations prior to use. Referenced Documents .1 ASTM Standards: 4193 Specification for Reagent Water2 2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings3 D 3335 Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption - Spectroscopy3 >3618 TestMethod for Detection of Lead in Paint and Dried Paint Films3 `iimmary of Test Method .1 A weighed quantity of the paint sample is diluted , vent-reducible paints in methyl isobutyl ketone and ter-reducible paints in water) and then aspirated into the j'er of an atomic absorption spectrometer. Lead content the paint is determined from a calibration plot of rbance versus concentration, prepared from standard "ings containing known amounts of lead. ignifieance and Use ll Current U.S. regulations restrict the amount of lead '"t may be present in consumer paint products to less than 6 % based on the total solids. This test method provides a rapid means for screening paints to, determine compliance with those1 regulations. The test method may be adjusted to meet regulations with a different limit on lead content. 5. Apparatus 5A 'Atomic Absorption Spectrophotometer, consisting, of an atomizer and either a single- or a three-slot burner, gas pressure, regulating and metering devices for air and acety lene, lead source lamp with a regulated constant-current supply, a monochromator and associated optics, a photosen sitive detector connected to an electronic amplifier, and a readout device. 5.2 Volumetric Flasks, 50 mL.' 6. Reagent and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be used in all tests unless otherwise specified. Unless otherwise indicated, it is intended that'all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where'such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determi nation. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water conforming to Type II of Specification D 1193. 6.3 Methyl Isobutyl Ketone (MIBK), technical grade. 6.4 Standard Paints--Prepare at least 3 standard paints by adding; accurately weighed quantities of an analytically assayed compatible lead compound to a solvent-reducible or water-reducible paint that has been analyzed by Test-Method D3335 and shown to contain less than 10 ppm of lead. Determine the nonvolatile content of the base paint and choose quantities of the lead compound sp that the lead concentrations of the standard paints will be approximately 300, 600, and 900 pg/g based on the nonvolatile content. 7. Calibration and Standardization 7.1 Prepare at least three solvent-reducible or waterreducible standard paint specimens (see 6.4) that bracket the expected lead concentration in the sample to be tested. Following the procedure in 8.2 dilute the standards for aspiration. .This test method is under the jurisdiction of ASTM Committee D-l on Paint Related Coatings and Materials and is the direct responsibility of Subcom- D01.21 on Chemical Analysis of Paints and Paint Materials. ^-urrent edition approved Dec. 16, 1988. Published February 1989. 'Annual Book ofASTM Standards, Vols 06.03 and 11.01. Annual Book ofASTM Standards, Vol 06.01. 4 Reagent Chemicals, American Chemical Society Specifications, Am. Chem ical Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see "Reagent Chemicals and Standards," byJoseph Rosin, D. Van Nostrand Co.. Inc., New York, NY, and the "United States Pharmacopeia." 857. md DUP050298037 # D 4834 7.2 Operational instructions for atomic absorption spectrophotometers vary with different models. Consult the manufacturer's literature for establishing optimum condi tions for the specific instrument used. 7.3 Turn the instrument on and set the wavelength to the 283.3-nm lead line. Apply the current recommended by the manufacturer to the lead source lamp. Allow the instrument to warm up for about 15 min and set the slit width. Adjust the air and acetylene pressure or flow rates and ignite the burner in accordance with the manufacturer's instructions. A background corrector should be used. 7.4 Aspirate each of the diluted standard paints and record the corresponding absorbance readings. Aspirate MIBK or water, as appropriate, between standards. N' 1; Caution--it is important that MIBK or water be aspirated immediately after each diluted standard paint to minimize fouling ofthe aspirator/nebulizer system which could change the aspiration rate and absorbance reading. Continued response for lead while aspirating MIBK or water may indicate contamination of the burner head with pigment and require cleaning of the burner head. N' 2--To be certain that the diluted paint specimen remains homogeneous during aspiration, the flask containing the specimen may be stirred continuously with a small magnetic stirring bar. 7.5 Construct a calibration curve on linear graph paper by plotting the absorbance readings versus micrograms of lead present in each diluted standard paint as follows: A = (B x D x E) where: A = lead present, jug, B = lead in standard paint based on nonvolatile content (see 6-4), ng/g, D = weight of standard paint, g, and E = nonvolatile portion of standard paint, %. 8. Procedure 8.1 Mix the paint to be tested until homogeneous, prefer ably on a mechanical shaker. Determine the nonvolatile content in accordance with the appropriate test method selected by consulting Guide D 2832. 8.2 Prepare at least two replicate specimens by weighing by difference from a weighing bottle or disposable syringe to 0.1 mg, 0.5 0.02-g quantities of the paint being tested, into 10 raL volumetric flasks. Dilute to the mark with MIBK, if the paint is solvent reducible, or with water, if it is water reducible. Mix thoroughly. N' 3--Adjustment of specimen size and dilution volume may be made as required for linear calibration and reasonable response for the instrument used as well as for differing lead content limits. 8.3 Aspirate the diluted paint specimens immediately (Caution--Sec Note 1) after mixing and measure the absorbance (see Note 2). Aspirate MIBK or water, as appropriate between specimen aspirations. Determine the micrograms of lead present from the calibration curve. N ' 4--For maximum accuracy, calibration and standardizaun (See Section 7) should be completed just prior to aspirating the dilute paint specimen. 0 9. Calculation 9.1 Calculate the mean concentration of lead in the nonvolatile portion of the paint specimen as follows: L=(Cx 100)/{AVxS) where: L = lead in nonvolatile portion of the paint specimen!! ppm (pg/g), C = lead in the aspirated specimen solution (8.3), gg, Jjl 100 -- factor derived from multiplying the numerator by>1 100 (to convert NVused to a whole number) and lb1 (to obtain ppm) and multiplying the denominator by 106 (to convert grams of specimen to micrograms), ' NV = nonvolatile portion of paint specimen, %, and 5 = weight of specimen, g. 10. Report 10.1 Report the lead concentration expressed on thffj nonvolatile content of the paint sample. 11. Precision and Bias5 11.1 Precision--The precision estimates are based onf interlaboratory study in which five different laborno: i analyzed in duplicate on 2 days, three samples of sober..-. ' reducible paints and three samples of water-reducible paintff containing from 464 to 742 ppm lead. The within-laboratory! coefficient of variation was found to be 3.34 % relative at df and the between-laboratories coefficient of variation w-.x" 6.72% relative at 18 df. Based on these coefficients, thel following criteria should be used forjudging the acceptobilr.;^ of results at the 95 % confidence level: 11.1.1 Repeatability--Two results, each the mean of du plicate determinations, obtained by the same opera oi <, fc different days should be considered suspect if they differ h 1 more than 9.76 % relative. | 11.1.2 Reproducibility--Two results, each the mean ofl duplicate determinations, obtained by operators in different;! laboratories should be considered suspect if they differ b;' more than 19.96 % relative. 11.2 Bias--Bias is under investigation. `1 12. Index Terms 12.1 This test method is indexed under the following terms: spectroscopy--atomic adsorption; lead content-q4r paint; lead screening test. 5 Supporting data is available from ASTM Headquarters. Request RR: I 1060. V The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard ate expressly advised that determination of the validity oi any such patent rights, and the risk ot infringement of such rights, are entirely their own responsibility. This standard is subject fo revision at any time by the responsible technical committee and must be reviewed every five years and It not revised, either reapprovedor withdrawn. Your comments are invited either for revision ot this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you shoutd make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 858 DU PO50298038 Designation: D 4838 - 88 Standard Test Method for Determining the Relative Tinting Strength of Chromatic L Paints1 This standard is issued under the fixed designation D4838; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A k superscript epsilon (e) indicates an editorial change since the last revision or reapproval. Scope 1.1 This test method describes the determination of the ibsorption tinting strength of a chromatic test paint relative 3 that of a standard or reference paint of the same chemical . The procedures are based on dilution of the paints with |standard mixing white paint, followed by instrumental ieasurement and calculation. Provision is made for cor- iting the results for small differences in hue or chroma, or oth, between the test and reference chromatic paints. .2 This test method is intended for the comparison of (tits containing the same type of vehicle (acrylic, alkyd, or and single-pigment colorants of the same Colour Index2 le and number. The amounts of the pigment and of the :her components of the paint need not be known. 1.3 This standard may involve hazardous materials, opertions, and equipment. This standard does not purport to iress all ofthe safety problems associated with its use. it is <e responsibility of the user of this standard to establish vopriate safety and health practices and determine the ijicabilily ofregulatory limitations prior to use. Referenced Documents |ki ASTM Standards: : D1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature3 % D 4303 Test Methods for Lightfastness of Pigments Used in Artists' Paints3 |E 284 Definitions of Terms Relating to Appearance of Materials"' ! 308 Method for Computing the Colors of Objects by Using the CIE System4 jpE 1164 Practice for Obtaining Spectrophotometric Data for Object-Color Evaluation4 ' Terminology ;3.1 Definitions: ?'3.1.1 tinting strength--measure of the effectiveness with hich a unit quantity of a colorant alters the color of a laterial. For scattering and absorbing colorants (pigments). UTllis test method is under the jurisdiction of ASTM Committee D-i on Paint ^Related Coatings and Materials and is the direct responsibility of SubcomHitfie D01.57 on Artist Paints and Related Materials. |iCurrcnt edition approved June 24, 1988. Published November 1988. tfCohur Index, The Society of Dyers and Colourists, London, 1987. Available totn the American Association of Textile Chemists and Colorists, P.O. Box 12215, 'search Triangle Park, NC 27709. E/tnnual Book ofASTM Standards, Vol 06.01. f.AnnUGl Book ofASTM Standards, Vo] 14.02. both absorption and scattering tinting strength must be specified. 3.1.2 tinting strength, absorption--relative change in the absorption properties of a standard white material when a specified amount of an absorbing pigment, black or chro matic, is added to it. D< ( < --This is the common definition of tinting strength; however, this definition of the term can be mis leading. For example, the tinting strength of a yellow colorant depends on its scattering as well as its absorption. Its tinting strength as determined from a mixture with white provides no information about its behavior when mixed with low-scattering colorants, such as a black. 3.1.3 tinting strength, scattering--relative change in the scattering properties of a standard black material (with no white pigment present) when a specified amount of a white or chromatic scattering pigment is added to it. 3.1.4 For other definitions, see Definitions E 284. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 drawdown--a layer ofpaint deposited on a substrate by use of a drawdown bar to evaluate the characteristics of the paint.. 3.2.2 drawdown bar--a bar designed to deposit a specified thickness of wet paint film uniformly on a specified test panel or other substrate. 4. Summary of Test Method 4.1 Chromatic paints are diluted with white paint to obtain mixtures that will produce a drawdown having 35 to 45 % reflectance factor at the wavelength of maximum absorption, 4.2 Drawdowns of these mixture paints are produced at complete hiding. 4.3 The drawdowns are measured, to obtain tristimulus filter readings A, G, B either directly or by computation from CIE tristimulus values X, Y, Z. 4.4 One ofthe samples is designated the standard, and the percents of tinting strength, % TS, of the others are calcu lated relative to that of the standard. Provision is made for correcting this tinting strength for small differences in hue, chroma, or both, between the standard and the test spec imen, and for obtaining an average tinting strength and a range. 5. Significance and Use 5.1 Tinting strength may be one factor in judging the relative economic value of paints, since pigment concentra tion contributes to strength in a major way; other factors are formulation and color development in grinding. The user may also select products for other properties, such as 859 DUP05 02 98039 transparency, that are accompanied by different tinting strengths. The results of this test method may be used for production control or quality comparisons. 5.2 The product with the greatest or the least tinting strength may not be the most desirable for a given artistic use. For example, low tinting strength may lead to the need to use an excessively high pigment concentration to obtain a desired color effect, and this may lead to defects in the dry paint film. 5.3 This test method applies only to single-pigment paints. The tinting strength of paints that contain two or more chromatic pigments with different optical properties cannot be evaluated by this test method. 5.4 The term "similar chemical type" used in 1.1 does not limit the ingredients in the paints to identity, but refers to compatibility in the case of vehicles and to: similarity in the case of pigment types. 5.5 While the instrumental evaluation of tinting strength is described, visual comparisons can also be used, with lower precision, and should be made to provide confirmation of the instrumental and computational results. 5.6 If the sample and standard are widely different in appearance when prepared at the same ratio of chromatic to white paint, another sample should be prepared to bring the two closer in appearance, to obtain the most accurate results. 5.7 The quantities, of chromatic and white paints mixed must be accurately known, on either, a weight , or a volume basis, but the concentration of pigment in the chromatic paint need not be known. 5.8 When the paints being compared have the same vehicle and pigment (same Colour Index name and number) the values of uncorrected tinting strength from 9.1 and corrected tinting strength from 9.2 should be nearly the, same. If they are not, an average of the two tinting strengths is recommended as the best estimate of the true value, and a range provides a measure of the magnitude of the uncer tainty, which is due to differences in hue or chroma, or both, between- the paints. 5.9 Strictly speaking, the Kubelka-Munk-type analysis of this test method should not be applied to the tristimulus filter readings used, but only to spectral data. For the purposes of the relative comparisons of this test method, however, the errors introduced by the calculations used cancel to an adequate degree. 6. Apparatus and Materials 6.1 Laboratory Balance, top-loading, having a sensitivity of 0.01 g. 6.2 Drawdown bars, capable of producing smooth paint films with wet-film thicknesses between 0.003 and 0.010 in. (0.075 and 0.25 mm).5 6.3 Opacity charts, sealed-paper type with black and white areas.6 6.4 Color-Measuring Instrument, either a spectrophotom eter providing 1931 CIE tristimulus values X, Y, Z for CIE 5 Suitable drawdown bars can be obtained from the Paul N. Gardner Company, Inc., P.O. Box 10688, Pompano Beach. FL 33061-6688, or BYK-Gardncr, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. *' Leneta 2A charts, available, from the Leneta Co., Box 576, Ho-HoKus, NJ 07423, and the Morest Co., 2) I Center St., New York. NY 10013, have been found satisfactory for this purpose. standard illuminant C, or a tristimulus colorimeter providing either such tristimulus values or colorimeter readings R c, I B. ' '"a 6.5 Mixing While Paint, prepared as described in the Specimen Preparation, Mixing Whites for Dilution of Colon section of Test Method D4303. Alternatively, a commercial titanium-dioxide white artists' paint may be used. Th mixing white paint must be made with the same vehicle tyi (acrylic, alkyd, or oil) as the paints to be tested. 7. Specimen Preparation 7.1 Obtain representative samples of the chromatic pr.i, to be tested. For tube paints; expel the entire contents ol il tube and mix thoroughly before sampling. 7.2 Determine the approximate amount of chromat paint to be added to 20 g of mixing white paint to obtain drawdown with 35 to 45 % reflectance factor at the wav length of maximum absorption. If the amount of chromat paint is not known in advance, consult the tables Appendix X1. For pigments other than those listed, use the general guideline the addition of 5 g of chromatic pa, containing an inorganic pigment or 1 g of chromatic pai. containing an organic pigment to the 20 g of miking whi paint. N' 1--Appendix Xi of Test Method D 4303 describes a methi for computing the necessary adjustments in quantities required additional trials arc needed to obtain the desired level of reftectaa factor. 7.3 Weigh out the chromatic and mixing white paints the nearest 0.01 g, and mix thoroughly. 7.4 Prepare drawdowns by placing the paint mixtui: one end of an opacity chart and pulling the drawdown b. smoothly through the paint and across the chart. Paste pain should ,be spread with a spatula or palette knife over t! entire chart area to be covered before pulling the bar dots the chart. 7.5 Allow the drawdowns to reach the dry-to-touch tirr as described in the Procedure section of Test Metbe D 1640. Acrylic paints should dry in air overnight. Ajkj paints may require 5 days to dry. Oil paints may require months to dry. 7.6 Determine whether each drawdown is at completi1 hiding by measuring the portions of it over the black and over the white areas of the chart to determine tristimul value Y or colorimeter reading G. If the quotient YJYv, Ge/Gw, where the subscripts refer to measurements c black and white, respectively, is greater than 0.98, fire drawdown can be considered at complete hiding. If the' drawdown is not at complete hiding, prepare a thickr$! drawdown or a drawdown made with multiple coats ofpainty one over another. N' 2--At the required dilution with while, a drawdown bar with an aperture of 0.006 in. (0.15 mm) will usually make a drawdown at' complete hiding. In the eases of some acrylic paints and a few oil pamls it may be necessary to increase the aperture to 0.010 in. (0.25 mm) to obtain complete hiding. If this leads to a slow-drying film or a film I > is wrinkled when dry, multiple coats can be applied by depositing ?second 0.006 in. (0.15 mm) coat, drawing down at a right angle to the first coat. After this coat dries, a third coat can be applied if necessart by using a shorter bar that rides over the previous coats. 860 DUP050298040 # D4838 . Procedure 8.1 Obtain values ofR, G, B for each sample by either of ne two following procedures. 8.1.1 Measure the drawdown with a spectrophotometer or tristimulus colorimeter to determine 1931 CIE tristimulus alues X, Y, Z for CIE standard illuminant C. Follow 'ractice E 1164 and Method E 308. If hemispherical (interating-sphere) geometry is used, measure with the specular omponent excluded. 8.1.2 If a colorimeter that is direct reading in >R, G, B is ised, measure these quantities. 8.2 If X, Y, Z are measured, calculate R, G, B by use of he following equations: R - 070.98 - 0.2Z/I.l8)/0.8 (1) G= Y (2) B = Z/1.18 (3) N' 3--The use of the 1931 CIE system (and standard observer) nd standard illuminant C is specified because all known tristimulus olorimeters that are direct reading in R, G, B measure for these onditions. If values of X, Y, Z are obtained by spectrophotometry, the 964 CIE system and other CIE standard illuminants may be used. Equations 1 to 3 are specific to the conditions, and must be replaced by be appropriate equations if other conditions are specified.7 The article Jsferenced also discusses correcting the measured values for surface Elections. I Calculation | 9.1 Calculate uncorrected relative tinting strength, % tSuc as follows: 9.1.1 Using decimal-fraction values of R, G, B, calculate Cubelka-Munk-type ratios of absorption coefficient, K, to cattering coefficient, S: (A-/S)*=(l -RfjlR(AT/S)C=(1 -Gf/IG (K/'S)B = <1 - BfjlB (4) (5) (6) 9.1.2 Calculate the pigment concentration term C,;. CP = QJ(QC + QJ vhere: = quantity of chromatic paint, g, 2W = quantity of white paint, g. (7) N' 4--If it is desirable to use volume rather than weight as the lasis for comparison of tinting.strengths, determine the densities of the faints and compute the volumes of the weighed samples. Calculate CP ty use of Eq 7 using volumes instead of weights. 9.1.3 Calculate normalized values of (K/S), denoted N, as ollows: Nr = (K/S)r /Cp (8) Na " (KIS)g ICp (9) Nb = (K/S)b/Cp (10) 9.1.4 Select one of the specimens to be denoted the standard and assigned the value of 100 % tinting strength. The tinting strength of the remaining specimens will be determined relative to that of the standard. 9.1.5 Select the value of N to be used in the calculation of % TSUC by one of the following three methods: 9.1.5.1 Select N based on the visually determined color of the specimen: For blue and green specimens, select NR, for purple and red specimens, select NG\ and for yellow and orange specimens, select NB. Relabel the selected value TVI' ( and IV" fc>r the specimens and the standard, respectively. Relabel the remaining two values of N as Nls?nc an<3 NS' ( fr the specimens and N2STD and Ar3STD for the standard. 9.1.5.2 If the specimen color cannot be classified accu rately in 9.1.5.1, select the lowest value ofNas M. The same selection must be made for the standard and all specimens to be compared. Relabel the values of A'as in 9.1.5.1. 9.1.5.3 If the values of NR and NB for the specimen are both low and approximately equal, follow the procedure in Annex A1 to select N and calculate the tinting strength. 9.1.6 Calculate % TSUC as follows: % TSVC = 100 (M' ( /M " ) (U) 9.2 Calculate tinting strength corrected for differences in hue and chroma, % TS& by use of the following equations: ^SPEC ** ^SPEC "l" ^SPEC ^STD " + 1V3" O =s (^SPEC ^ST" )/2 % TSC = 100 (M' ( - TOAVlsro (12) (13) (14) (15) 9.3 Calculate average tinting strength, % TSAV, and range E as follows: % TSAV = (% TSVC + % TSc)/2 (16) E - (% TSUC - %TSc)/2 (17) 10. Report 10.1 Report the following information: 10.1.1 Complete identification of the specimens, in cluding brand and color name, date of manufacture, and lot number if available. 10.1.2 Name of color-measuringinstrument used, method of standardization, and other information required in the Report section of Practice E 1164 and Methods E 308. 10.1.3 Date oftest. 10.1.4 Test results for % TSVC, % TSC, or % TSAV, and range. 11. Precision and Bias8 11.1 Based on interlaboratory intercomparisons, the re sults ofthis test method agree to within +6 % on an absolute basis. 12. Index Terms 12.1 This test method is indexed under the following terms: artists' paints; chromate coatings; tinting strength. 7 Johnston-Feller, R. M., and Bailie. C W., "Determination or the Tinting Strength of Chromatic Pigments," Journal of Coalings Technology, Vol 54, No. S92, 1982, pp. 43-56. --------------------------- a Supporting data are available from ASTM Headquarters. Request RR-.DQ I 1057. 861 DUP050298041 # D 4838 ANNEX (Mandatory Information) Al. Procedure for Pigments with Two Separated Absorption Maxima Al. The tinting strength of pigments, such as chromium oxide green, for which both Nn and NB are low and approximately equal, must be calculated by the following equations: NUM -- ' ( t" N' .' ( V2 DENOM = (Nr s t d + Nbstd)/2 ~ (^{ .' ( + NasrD)/2 % TSUC = 100 NUM/DENOM ' % TSC = (NUM - Z))/DENOM (A: ' (A: 2 (Al 3) (A: ,| (A- ISi i j t SU! APPENDIX (Nonmaiidatory Information) TABLE XI.1 Approximate Weight of Acrylic Paint to Mix With 20-g of Mixing White Paint Pigment Name Colour index Name Chromatic Paint, g Alizarin crimson. Azo yellow medium Burnt umber Cadmium-barium orange Cadmium-barium red medium Cadmium-barium yellow, fight Cadmium-barium' yellow medium Cerulean blue Co-Cr Cerulean blue Co-Sn Chromium oxide green Cobalt blue Dioxazlne purple Bansa yellow light Naphthol AS-OL red Naphthol red light AS-D Phthalocyanine blue Phthalocyanine green Raw sienna Raw umber Red oxide , Ultramarine bide Yellow oxide ' PR 63 PY 74 PBr 7 PO 20:1 PR 108:1 PY 35:1 PY 37:1 PB 36; PB 35 PG 17 PB 28 PV 23 RS PY 3 PR 9 PR 14 PB 15 PG 7, PG 35 PBr 7 PBr 7 PR 101 PB 29 PY 42 2.5 2.5 3.0 2.5 4.0 4.0 3.3 9.0 10.0 4.0 5.0 1.0 3.0 2.5 2.0 0.4 0.5 4.0 6.0 1.0 4.0 4.0 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and tha risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 862 DUP050298042 Designation: D 4839 - 88 Standard Test Method for Total Carbon and Organic Carbon in Water by Ultraviolet, or Persulfate Oxidation, or Both, and infrared Detection1 This standard is issued under the fixed designation D 4839; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. pcope ... .: |;;'l This test method covers the determination, of,-total bon (TCI, inorganic carbon (IC), and total organic carbon OC) in water, wastewater, and seawater in the range from 1 mg/L to 4000 mg/L of carbon. - ";,2 This test method was used successfully with reagent ter spiked with sodium carbonate, - acetic acid, and ridine. It is the user's responsibility to ensure the validity Shis test method, for waters of untested matrices. i.3 This test method is applicable only to carbonaceous atter in the sample that can be introduced into the reaction fejThe syringe needle or injector opening size generally it the maximum size of particles that can be so intro- ced. : 1.4 In addition to laboratory analyses, this test method may be applied to stream monitoring. . fey'This standard may involve hazardous'materials, bper- jims, and equipment. This standard, does not purport to dress all ofthe safety problems associated with, its use. It is . responsibility of the user of this standard to establish fopriaie safety and Health practices and determine the tfficability ofregulatory limitations prior id use. Referenced Documents 2.1 ASTM Standards: D i 129 Terminology Relating to Water2 D11S2 Specification for Equipment for Sampling Water and Steam2 *,D 1193 Specification-fbr.Reagent Water2 -D2777 Practice for Determination of Precision and Bias of Applicable Methods of Committee D-19 on Water2 D 3370 Practices forSatnpling Water2 ISD 4210 Practice for Intralaboratory Quality Control Pro cedures and a Discussion on Reporting Low-bevel ..--Data2 - . Terminology ' 3.1 Definitions: 3.1.1 For definitions of terms used in this test method, fer to Specification D 1129. fill Description of Terms Specific to This Standard: . 3.2.1 inorganic carbon (IQ--carbon in the form of bon dioxide, carbonate ion, or bicarbonate ion. 1 This test method is under the jurisdiction of ASTM Committee D-19 on Whter aiid is the direct responsibility of Subcommittee D 1-9.06 on Methods for \ felysis for Organic Substances in Water. ^Current edition approved June 24, 19B8. Published September 1988. 2 Annua! Book ofASTMStandards, Vol (1.01. 3.2.2 total organic carbon (TOQ--carbon in the form of organic compounds. , 3.2.3 total carbon (TQ--the sum of IC and OC. 3.2.4 refractory material--that which.cannot be oxidized completely under the test method, conditions. 4. Summary of Jest Method 4.1 Fundamentals--Carbon can occur in water as an inorganic and organic compound. This test method can be used to make independent, measurements of IC, TOQ and TC, and can also determine IC by the difference of TC and TOC, and TOC as the difference of TC and IC. , 4.2 The essentials of this test method are: (a) removal of IC,. if desired, by acidification of the sample and sparging by carbon-free gas; (b) conversion pf remaining carbon to CQ2 by action of persulfate, aided either by elevated temperature or ultraviolet (U.V) radiation; (c) detection; of C02 that is swept out .of the. reactor by a gas stream; and (d), conversion of detector signal to a display of carbon concentration in mg/L, A diagram, of suitable apparatus is given in Fig. 1. 5. Significance and Use . jt 5.1 This test method is used for determination of the carbon content of water from a variety ofnatural, domestic, and industrial sources. In its most common form, this test method is used to measure organic carbon as a means of monitoring .prganic pollutants in industrial wastewater. These measurements are also used in monitoring waste treatment processes. 1 5.2 The relationship of TOC to other water quality parameter^.such as chemical oxygen demand (COD) and total'Oxygen demand (TOD) is described in the literature.3 6. Interferences and Limitations 6.1 The oxidation of dissolved carbon to C02 is brought about at relatively, low temperatures by the chemical action of reactive species produced by hot or UV-irradiated persulfate ions. Even-if oxygen is used as the sparging gas, it makes a much lower contribution to, oxidation than in high-temperature (combustive) systems. Not all suspended or refractory material may be oxidized under these condi tions; analysts, should take steps to determine what recovery is being obtained. This may be done by several methods: (a) by monitoring reaction progress to verify that oxidation hasbeen completed; (b) by rerunning the sample under more vigorous reaction conditions; (c) by analyzing the sample by 3 Handbook for Monitoring Industrial IVastewater, Section 5.3. U.S. Environment Protection Agency, August 1973, pp. 3-12. 863 DUP050298043 D 4839 REAGENT SUPPLY SAMPLE SUPPLY REACTION VESSEL GAS DEMISTER & DRYER r H co2 TRAP \ (OR) < j-. / NDIR C02 DETECTOR FIG. 1 Diagram of Apparatus CONTROL MODULE DISPLAY PRINTER an alternative method known to result in full recovery; or (d) by spiking samples with known refractories and determining recovery. 6.2 Chloride ion tends to interfere with oxidative reaction mechanisms in this test method, prolonging oxidation times and sometimes preventing full recovery. Follow manufactur er's instructions for dealing with this problem: See Appendix X1 for supporting data. 6.3 Homogenizing or sparging of a sample, or both, may cause loss of purgeable organic compounds, thus yielding a value lower than the true TOC level. (For this reason, such measurements are sometimes known as nonpurgeable or ganic carbon (NPOC)). The extent and significance of such losses must be evaluated on an individual basis. This may be done by comparing the TOC by difference (TC-IC) with the direct TOC figure, that is, that obtained from a sparged sample. The difference, if any, between these TOC figures represents purgeable organic carbon (POC) lost during sparging. Alternatively, direct measurement of POC can be made during sparging, using optional capabilities of the analyzer. 6.4 Note that error will be introduced when the method of difference is used to derive a relatively small level from two large levels. For example, a ground water high in IC and low in TOC will give a poorer TOC -value as (TC-IC) than by direct measurement. 7. Apparatus 7.1 Homogenizing Apparatus--A household blender is generally satisfactory for homogenizing'immiscible phasesin water. .' 7.2 Sampling Devices--Microlitre-to-millilitre syringes are typically required for this test method. Alternatives include manually operated or automatically operated sam pling valves. Sampling devices with inside diameters as small as 0.15 mm may be used with samples containing little or no particulate matter. Larger inside dimensions such as 0.4 mm will be required for samples with particulate matter. N' 1--See 6.1 concerning oxidation of particulate matter. 7.3 Apparatus for Carbon Determination--This instru ment consists of reagent and sample introduction mecha nism, a gas-sparged reaction vessel, a gas demister or dryer, or both, an optional C02 trap, a C02-specific infrared detector, a control system, and a display. Fig. 1 shows a diagram of such an arrangement. 7.3.1 Sparging requires an inert vessel with a capacity of at least double the sample size with provision for sparging with 50 to 100 mL/min of carbon free gas. This procedure will remove essentially all IC in 2 to 10 min, depending on design. 7.3.2 Oxidation--The reaction assembly contains reagent and sample introduction devices, and a reactor vessel with sparging flow ofcarbon-free gas. The vessel may be heated by an external source, and may contain a UV lamp. The reaction vessel and sparging vessel (see 6.3.1) may be combined. 7.3.3 Gas Conditioning--The gas passing from the reactor is dried, and the C02 produced is either trapped and later released to the detector, or routed directly to the detector through a chlorine-removing scrubber. 7.3.4 Detector--The C02 in the gas stream is detected by a COrspecific nondispersive infrared (NDSR) detector. 7.3.5 Presentation ofResults--The NDIR detector output is related to stored calibration data and then displayed as milligrams of carbon per litre. s 8. Reagents and Materials 8.1 Purity ofReagents--Reagent grade chemicals shall h; used in all tests. Unless otherwise indicated, it is intended that all reagents conform to the. specifications of the Com mittee on Analytical Reagents of the American Chemical Society,4 where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficient purity to permit its use without lessening the accuracy of the determination. , 8.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water, conforming to Specification D 1193, Type I or Type 11 'I he indicated specification does not actually specify inorganic carbon or organic carbon levels. These levels can affect the results of this test method, especially at progressively lower levels of the carbon content in the samples to be measured? Where inorganic carbon in reagent water is significant; C02-free water may be prepared from reagent water by acidifying to pH 2, then sparging with fritted-glass sparger using COz-free gas (time will depend on volume and gas flow rate, and should be determined by test). Alternatively, if the carbon contribution of the reagent water is known accu rately, its effect may be allowed for in preparation of standards and other solutions. C02-free water should be protected from atmospheric contamination. Glass containers are required for storage of water and standard solutions. , 8.3 Acid--Various concentrated acids may be used for acidification of samples and of the oxidizing reagent. Acids such as phosphoric (sp gr 1.69), nitric (sp gr 1.42), or sulfuric (sp gr 1.84) are suitable for most applications. Sulfuric acid 4 "Reagent Chemicals, American Chemical Society Specifications,'* Artterican Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the A.C.S., see "Reagent Chemicals and Standards," by Joseph Rosin, D. Van Nostrand Co.. Inc, New York, NY and the "United Slate Pharmacopeia." 864 DUP050298044 pi | # 0 4839 I be used in the form of a 1 + 1 dilution, for safety asons. Hydrochloric acid is not recommended. f 8.4 Organic Carbon, Standard Solution (2000 mg/L)-- Choose a water-soluble, stable reagent grade compound, |uch as benzoic acid or anhydrous potassium hydrogen ghthalate (KHC8H404). Calculate the weight of compound inquired to make 1 L of organic carbon standard solution; fbr example, KHCgH404 = 0.471 g of carbon per gram, so t|ne litre of 2 g/L ofstandard requires 2/0.471, or 4.25, grams iff KHP. Dissolve the required amount of standard in some p02-free water in a 1-L volumetric flask, add I mL of acid, fed dilute to volume. This stock solution, or dilutions of it, fay be used to calibrate and test performance of the carbon (ftalyzer. 8.5 Persulfate Solution--Prepare by dissolving the appro bate weight of potassium or sodium persulfate in 1 L of ater, to produce the concentration specified by the instru ment manufacturer. If specified, add 1 mL of phosphoric Kid (sp gr 1.69) and mix well, Store in a cool, dark place, teeipes for this reagent solution may be modified by manufacturers to meet the needs of specific applications, for ;kample, high chloride samples. 8.6 Gas Supply--A gas free of C02 and of organic matter -required. Use a purity as specified by the equipment anufacturer. The use of oxygen is preferred for the UVIrsulfate method, and nitrogen or helium is preferred if a X>2 trap is used between reactor and detector. 9. (Sampling and Sample Preservation p.9.1 Collect the sample in accordance with Specification >1192 and Practice D 3370. ^9:2 To preserve Samples for this analysis, store samples in jjla^s at 4C. To aid preservation, acidify the samples to a pH (flUIt should be noted that acidification will enhance loss of jffjrganic carbon. If the purgeable organic fraction is imporJjBtt, fill the sample bottles-td overflowing vnth a minimum pf turbulence and cap them using a fluoropoiymer-lined cap, Jdtjhout headspace. Jr:3 For monitoring of waters containing solids or immisble liquids that are to be injected into the reaction zone, use Prhechanical homogenizer or ultrasonic disintegrator. Filjjgtihg or screening may be necessary after homogenization to ijeet particle sizes that are too large for injection. Volatile panics may be lost. See 6.3. 1914 For wastewater streariis where carbon concentrations (greater than the desired range of instrument operation, tlute the samples as necessary. |l Instrument Operation 10.1 Follow the manufacturer's instructions for instruaent warmup, gas flows, and liquid flows. Calibration 11.1 Use the stock solution of 2000 mg/L of carbon, and arious dilutions of it, for calibration. No t ' 2--Dilutions should be made with COj-free water (see 8.2). 11.2 Calibration protocols may vary with equipment nufacturers. However, in general, calibrate the instrument . accordance with the manufacturer's instructions, and use ndards to verify such calibration in the specific range of interest for actual measurements. Plots of standard concen tration versus instrument reading may be used for calibra tion or to verify linearity of response. 11.3 Establish instrument blank according to the manu facturer's instructions. 12. Procedure 12.1 Mix or blend each sample thoroughly and carry out any necessary dilution to bring the carbon content within range of the instrument. 12.2 If inorganic carbon is to be measured directly, inject the sample into the analyzer under appropriate conditions. 12.3 If inorganic carbon is to be removed by sparging prior to sample introduction, acidify to approximately pH 2 with concentrated acid (if not already done) and sparge with an appropriate flow ofgas. Samples with high alkali content or buffer capacity may require larger amounts of"acid. In such cases, incorporate this dilution into the calculation. If incomplete sparging of C02 from IC is suspected, sparge and analyze the sample and then repeat the procedure until appropriate conditions are established. In difficult condi tions, use of a fritted-glass sparger may help. 12.4 To measure TOC, inject an appropriate volume of the sample into the analyzer. If external sparging is required to remove IC, inject a sparged sample for the TOC measure ment See 6.3. 12.5 To measure TC, inject an appropriate volume of unsparged sample. 13. Calculation 13.1 Read carbon values directly from a digital display or printer, or both. ' 14. Precision and Bias5 14.1 Collaborative Test--This test method was evaluated by sending seven identical sample to each of ten laboratories and asking them to measure TOC and TC exactly in accordance with this test method. Three of the ten laborato ries did not make the TC measurement. One of the samples consisted of laboratory reagent water: The other six were of that water spiked to various levels with' acetic acid, pyridine, arid sodium carbonate. TC leivels ranged from 0.6 to 2 000 mg/L, and TOC levels from 0.3 to 1 700 mg/L. An Ftest at 95% confidence level showed no significant difference between the results of the five laboratories using UVpersulfate oxidation and those of the five laboratories using hot persulfate. Consequently, results were pooled for further analysis. 14.2 Removal of Outliers--Application of outlier tests specified in Practice-D 2777 - 85 resulted in the elimination of one laboratory's TC and TOC results. In addition, three laboratories did not perform the TC analysis, so the effective number of laboratories was six for the TC measurement. Five of their individual results were later eliminated by outlier test. In the TOC determination, one additional laboratory failed the outlier test, leaving a total of eight. Three individual results were later eliminated. 5 Supporting data are available from ASTM Headquarters. Request RR: D-19-I 130. 865 DU P050298045 D 4839 *, AMOUNT RECOVERED bapC/ll FIG. 2 Precision Versus Amount Recovered ,14.3 Precision--Separate determinations of precision were made for TC and TOC measurements: For TC: S, -- 0.03x + 0.3 S, = 0.0U + 0.2 For TOC:St = O.OSx + 0. ; S0 = 0.04x + 0.1 where: x = the recovered C concentration, mg/L, S, = overall precision, and Sa - single-operator precision. Fig. 2 shows a log-log plot of the overall and single-operator precision of all TC and TOC measurements not eliminated by outlier tests. 14.4 Bias--Fig. 3 plots "amount added" against "amount foUnd," with overall precision shown as an error bar. Bias significant at the 95 % level (student's t-test) is flagged. Water that was used as one ofthe samples is omitted, since no value equivalent to "amount added" is available. The contribution ofthe carbon in the water to the spiked samples was allowed for before analysis of bias. In general, bias is positive, with the values running from 1 % to 25 % of the amount added, with no particular pattern evident. Of the twelve bias measurements, ten were below 10 %. Users of this test method should make their own determination of bias, 14.5 Matrix Effects--Participants were asked to measure the TC and TOC levels in a water sample of their choice, and FIG. 3 Bias: Amount Added Versus Amount Recovered then to spike the sample with one of the study samples and to measure the sample again. The chosen samples were: sinf waste; DI water with KHP; soil solution; tap water witl. added IC; plant waste stream; synthetic sewage, and anion resin brine wash. TC recoveries averaged 86 % (range from 74 % to 92 %), and TOC, 82 % (from 47 % to 92 %). The negative bias, versus the positive bias noted in 14.4, can reflect incomplete oxidation of spiking compounds in the presence of other organics, errors introduced by sample handling, or other effects. In any event, no one matrix was studied in sufficient depth to provide an answer. Users ofthis test method should conduct their own experiments to determine recovery in their particular circumstances. 14.6 The quality assurance (QA)/quality control (QC) portion of this test method has not been completely estab-j lished at this time. It is the intent of Subcommittee D 19.06 ; that procedures be incorporated into this test method that: require a minimum level of QC. These procedures will I require, at minimum, a method startup check and ongoing ! performance' checks. The analysts performing this test! method will be required to measure their performance against the performance level achieved by the laboratories that participated in the ASTM round-robin study done on this test method. These formal QC procedures will bi i incorporated at such time as they have been officially accepted by the Society. See Practice D 4210. 866 DUP050298046 APPENDIX (Nonmandatory Information) XI RECOVERIES OF VARIOUS COMPOUNDS FROM CHLORIDE-CONTAINING SOLUTIONS WITH UV-PERSULFATE OXIDATION TABLE XI .1 Percent Recovery Analyte "'potassium nyarogen fii"phthalate rea jiiitethanol iicotinic acid yridine Proline rt-ButancI Acetic acid wucine Acetonitrile 90.5 101.1 91.0 88.6 86.0 74.3 66.5 64.7 5.0 101.2 97.9 9B.0 92.2 96.2 101.3 96.6 88.0 TABLE X1.2 Recoveries of Potassium Hydrogen Phthalate from Chloride-Containing Solutions Using Hot Persulfate Oxidation ppm of Carbon Recovery 200 .800 99.4 % 92.0% Xl.l Conditions--Inject into the instrument 200 pL of solution, containing 100 ppm of carbon in the form of the compound indicated plus 1.8 % of chloride ion. Take results at the completion of oxidation or after 8 min, whichever occurs first. The American Society tor Testing and Materials takas no position respecting the validity ot any patent rights asserted in connection with any Item mentioned In this standard. Users ot this standard ere expressly advised that determination of the validity of any such patent rights, and the risk ot Infringement ot such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reappro/ed or withdrawn. Your comments are Invited eithar for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your Views known to the ASTM Committee on Standards. 1916 Race St., Philadelphia, PA 19103. fii 867 DUP050298047 d Designation: D 4938 - 89 Standard Test Method for Erosion Testing of Antifouling Paints Using High Velocity Water1 This standard is issued under the fixed designation D 4938; the number immediately following the designation indicates the year of original adoption o t , in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (c) indicates ao editorial change since the last revision or rcapproval. 1. Scope 1.1 This test method covers the determination of erosion rates for marine antifouiing paint systems immersed in flowing natural seawater. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 7. 2. Referenced Documents 2.1 ASTM Standards: ' A 569/A 569M Specification for Steel, Sheet and Strip, Carbon (0.15 Maximum Percent), Hot-Rolled, Com mercial Quality12 D823 Test Methods for Producing Films of Uniform' Thickness of Paint, Varnish, and Related Products on Test Panels3 D 1889 Test Methods for Turbidity of Water4 D2200 Pictorial Surface Preparation Standards for Painting Steel Surfaces3 2.2 US. Military Specifications:5 MIL-P-24441 Paint, Epoxy-Polyamide DOD-P-24647 Paint, Antifouling, Ship Hull (Metric) DOD-P-24655 Paint, Underwater Hull, Anticorrosion (Metric) 3. Summary of Test Method 3.1 Steel panels coated with the antifouling paint system under evaluation are positioned in a high velocity water channel, similar to the type shown in Figs. 1 to 3, parallel to the path of the flowing water. 3.2 Exposure conditions shall include at least one series of test panels evaluated at the standard water velocity of 12 m/s and shall specify the length of time, temperature, salinity, and pH. Additional velocities may be conducted at the discretion of the customer. 3.3 Color photographs and coating thickness measure- 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.45 on Marine Coatings. Current edition approved April 28, 1989. Published June 1989. 2 Annual Book ofASTM Standards, Vol 01.03. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vol 11.01. 5 Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. ments shall be taken prior to exposure, at specified liav ,=| intervals, and repeated at the end of the test for comparison m purposes. . jj 4. Significance and Use 4.1 This test method is intended to measure the erosion rates ofablative antifouling paint systems exposed to flowing water at velocities designed to subject the paint system to shear stresses experienced in service. 4.2 Measurement of erosion rates are necessary to help in the assessment of ablative antifouling paint film thickness required for fouling control between scheduled drydockinas , of ships, in the selection of materials, in producing quality * assurance, and in understanding the performance mecha-M nism. 4.3 The test data is intended to serve as a guide gggjj predicting the service life of ablative antifouling paintsItf'1' order to calculate the necessary paint thickness to fit' specified deployment cycles. Erosion rates of antifouling paints in service will vary depending on such factors ggjf berthing location, geographic area of operation, salinity, pH,' and temperature of seawater. It should also be recognize;a| that some areas of the ship are subject to different erosibflj rates. 4.4 The degree of correlation between results obtained! from this test method and shipboard service has not beeii|j determined. 5. Apparatus 5.1 Water Channel: 5.1.1 High velocity flowing water in a contained channe||| similar to the type shown in Figs. 1 to 3, is used to induce,, hydrodynamic shear stresses on painted panels to determinSf erosion rates of ablative antifouling paints. 5.1.2 The basic apparatus consists of a four-walleSI channel, rectangular in cross section, through which natunl seawater flows at varying linear velocities to simulate ship! ' speeds. 5.1.3 All wetted materials supplying seawater to and ! within the channel shall be nonmetallic with the following exceptions: 5.1.3.1 Channel circulating pump impellers. 5.1.3.2 Thermowells. 5.1.3.3 Channel flow orifice plate. 5.1.4 One section of the channel shall permit testing of the panels at a standard test velocity of 12 m/s. All sections of the channel shall provide flow with fully formed turbulent characteristics. A minimum Reynolds number of 1 000 000 shall be achieved in each velocity test section. The Reynolds number, R, is calculated as follows: 868 DUP050298048 D 4938 J? = (D X V X P)/U equivalent diameter = 4 x (area of flowing liquid/ wetted perimeter), m, velocity, in m/s, ,= density of medium, kg/m3, and = viscosity, P/s. a channel with a rectangular cross section and a test 1 placed in the middle of the channel, the equivalent eter would be calculated as follows: 4 X [(A X B)/{2A + 2B)] width of channel from side wall to panel face, m, and height of channel, m. 5.2 Erosion Rate Determination--Erosion rates of ablaantifouling paints are determined by using noneroding `nee points and measured in accordance with Section 8 the following equipment: 5.2.1 Microtome or encapsulating/polishing equipment. 5.2.2 Microscope with photomicrographic capability. .3 Seawater Requirements: 5.3.1 Seawater will be circulated through the channel at a ant rate permitting testing at different flow velocities as vain 9.3. 5/3.2 Natural seawater shall be continuously supplied to ; channel during operation to eliminate stagnation or -ntration effects, During operation of the channel the owing data shall be obtained and recorded on a daily sis: 5.3.2.1 Seawater circulating rate. 5 3.2.2 Seawater salinity and pH. 5.3.2.3 Incoming seawater temperature and the channel awater temperature. 5.3.3 Provisions shall also be made for supplying filtered Cawater to the channel. A suitable filter is one which can duce turbidity to Vz Jackson Turbidity Unit in accordance ith Test Method D 1889. 5.3.4 As a minimum, the seawater chemistry in the hannel, averaged over the course of the test run, shall be itliin the limits specified below: Maximum Minimum Salinity, ppm ptt 35 000 8.3 27 000 7.6 $5.4 Test Panels: 5.4.1 Steel test panels conforming to Specification A 569/ 569M shall be used in the channel. The panels shall easure 18.75 cm high, 15 cm long, and 1.25 cm thick. The Unted test panels shall be subjected to a double sided xposure with both sides exposed to similar hydrodynamic nditions. . 5.4.2 Test panels painted in accordance with Test `thods D 823 are positioned vertically and parallel to the wing water to simulate sheer stresses experienced by paints |i the ship's underwater hull. 5.4.3 The coating systems shall be applied in accordance jith the manufacturer's instructions for both the anti`rrosion and the antifouling paints. 5.5 Operation--The channel shall be operated on a con- fiuous basis during the test period except for downtime for Jnel inspection and seawater filtering system backwashes. The total running time of the test is defined as the total hours of actual channel operation under fully flowing conditions. 6. Application of Paints 6.1 Antifouling paints under evaluation may be applied by spray over a primer from the same manufacturer in accordance with the manufacturer's directions or over'9 mils of epoxy polyamide paint conforming to Military Specifica tion M1L-P-24441 with an appropriate tie-coat if necessary. Application shall be in accordance with Test Methods D 823. 7. Hazards 7.1 Antifouling paints contain toxic materials that could cause skin and eye irritation on contact and adverse physio logical effects if ingested or inhaled. In the preparation of , panels arid the application of various types of antifouling paints, the use of appropriate protective clothing and equip ment is required consistent with local, state, and federal government regulations and recognized industrial and tech nical standards. Spills, overspray, land unused material shall not be flushed down the drain but shall be disposed of as hazardous waste. 8. Procedure 8.1 Abrasive blast a minimum ofthree test panels for each system being evaluated to near-white metal, Sa 2Vi in accordance with Pictorial Standard D 2200, to obtain, a 1.0 to 3.0 mils (25. to 75 jj.m) surface profile. 8.2 Apply an epoxy anticorrosion primer in accordance with -Military Specifications >DD-P-24655 and MIL-P24441, or the manufacturer's recommendations, whichever applies. 8.3 Apply an antifouling topcoat in accordance with Military' Specification DOD-P-24647 or the manufacturer's recommendations, whichever applies. 8.4 Apply additional coats of antifouling paint in accord ance with Military Specification DOD-P-24647 or the man ufacturer's instructions, whichever applies. The last coat shall dry for a minimum of 7 days before any erosion testing. 8.5 Both sides of the painted test surfaces are provided with noneroding reference (NER) points before immersion in the test environment. The NER is an insoluble, tightly adherent vinyl or other suitable, compatible coating 2 0.5 cm/diameter applied in the center of the panel which will blanket a portion of the eroding surface. The NER preserves the original outer surface of the antifouling and thus offers a reference for comparison with the eroded surface during later microscopic examination. 8.6 Take film thickness measurements before and after testing (see 5.2). 8.7 Panels are to be photographed prior to starting the test for comparison with photographs taken at the conclusion of the test. 8.8 A specimen of exposed antifouling paint is carefully removed for examination in a single flake which includes a fragment of the noneroding reference. This specimen is mounted for microscopic analysis in a suitable medium such as paraffin wax or epoxy resin. Care is required to ensure that the specimen is not damaged by solvent attack or heat evolution during this encapsulation. 8.9 Specimens are prepared for examination by micro- 869 DUP0502 98049 D 4938 E < { . 1 High Velocity Flow Channel ( ' ourctt FJG. 2 TM/ig| ^IZ Kcj | IS M/Sfc. | ,e ware. ^ u --' G ( < msT ' ( <o n ---- Simplified Schematic of Flow Channel tome sectioning or by abrasive polishing to a plane surface. 8.10 Subsequent microscopic examination yields the typ ical image shown in Figs. 4 and 5. The material lost during the duration of the test is clearly shown as measurement d in Fig. 4. An actual photomicrograph is shown in Fig. 5. 9. Calculation 9.1 The material loss is expressed as the erosion rate ofthe ablative antifouling paint. 9.2 The erosion rate is calculated by dividing the mi crometers of surface erosion by the duration of the test expressed in months at a specified speed. STEEL. CHANNEL. T-80Lt L TEST PANEL i ACRYLIC PLATE . STL PLATE #> it d - - - f _> # : m... r i. 2M $ --C j/7 M FIG. 3 W, mm Velocity, m/s SO ' 60 75 100 150 300 18 15 12 9 6 3 Cross-Section View of Test Panel Mounted in Flow Channel (Low Velocity Section) 9.2.1 Example--A 20-pm erosion in 3 months equals 6.7 pm/month. 9.3 The speed of the water in the channel expressed in metres per second is correlated to a ship's speed expressed in 870 DUP0502 98050 D 4938 Nonpolishing Reference Polishing Coating Other Layers FIG. 4 Illustration of Material Lost During Testing lets in accordance with the following table: Channel, m/s 3 6 9 12 15 .18*' Speed, knots ! ' . -; 5.8 11.7 17.5 23.3 29.1 35.0 ' 9.3.1 Example--A typical erosiori rate is reported as 6.7' Vmonth at 17.5 knots, etc. ' h Report _ . ' r, " , ,'Y $0.1 The final test report shall include, the following data: $6.1.1 List of the paints tested, FIG. 5 Actual Microphotograph 10.1.2 Test duration--date started'and date ended, 10:1.3, Thickness readings before, aiid after exposure. Re port total paint film loss at the standard test velocity and any auxiliary test velocities, ,lfr 1,4' Daily, measurements of the seawater temperature, salinity, and the pH, , s, ' 10.1.5 Speed of test water, correlated to knots, 10.1.6 Observation of .the overall condition of painted panel, and 10.1.7 Initial and final photographs of the test panels. The American Society for Testing epri Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised Mat determination, of the validity of any such patent rights, and the risk of. infringement of.such rights, are entirely their own responsibility. This standard is subject to revision at anytlmo by the responsible technical committee and must be reviewed every five years and if pot revised, either reapprovedor.withdrawn. Your comments are invited either for revision of this standard or foradditional standards and should be addressed to .ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the AS.TM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 3 ;JS 'M jsj !>; 871 DUP0502 98051 Designation: D 4940 - 89 Standard Test Method for Conductitnetric Analysis of Water Soluble Ionic Contamination of Blasting Abrasives1 This standard is issued under the fixed designation D4940; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapprovat. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method describes a procedure for rapid evaluation of abrasives for the presence ofionic contamina tion by determining the total concentration of water soluble ionic contaminants by means of a conductivity test. 1.2 This test method does not identify the ionic species present nor provide quantitative results on each species. 1.3 This test method is based on a volume comparison among abrasives of similar sizes. A volume comparison is more closely related to surface area of the abrasives than is a weight comparison. 1.4 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1. Referenced Documents 2.1 ASTM Standards: D 1193 Specification for Reagent Water12 E 832 Specification for Laboratory Filter Papers3 3. Summary of Test Method 3.1 Abrasive and pure water are combined into a slurry that is stirred to leach the soluble salts from the abrasive. This slurry is filtered and conductance of the filtrate is measured. The conductivity, which is related to the concen tration of soluble ionic materials contaminating the abrasive surface, is calculated from the conductance and die cell constant. 4. Significance and Use 4.1 By-product abrasives manufactured from slags that are air cooled or quenched with pure water, normally contain low concentrations of ionic materials as do mined mineral abrasives. However, slags quenched with seawater or other contaminated water, contain high amounts of ionic material as does seashore sand. This contamination of the abrasive can transfer to the steel surfaces being blasted, where it may accelerate corrosion. This test is useful in establishing the cleanliness of the abrasive at the jobsite. 4.2 This test method provides a value that indicates the concentration of total water soluble ions in accordance wit i their electrolytic mobility. Thus, it provides an indication nl ionic corrosion potential. N' 1--A typical value of conductivity for a high level of contain. ination is 500 pmho/cm. A typical value for a low level of cantamination is 50 pmho/cm 5. Apparatus 5.1 Conductivity Bridge and Cell--Any commercial cor.ductivity bridge and conductivity cell having a range of at least 5 umho/cm to 1 000 000 (xmho/cm and temperature compensation capability is satisfactory. Either a dip-typ:, pipet-type, or cup-type cell may be used. A means of adjusting for temperature or controlling the temperature is essential. While some instruments have an adjustment to compensate for temperature, one means is to use a 25 C constant temperature bath. Another method is to stir ihe solution with a clean thermometer while the vessel is wanned or cooled by an external source. N' 2--If temperature compensation or control is not followed correctly, an error of approximately 2 % per degree of temperature deviation from 25C can be introduced. The deviation of conductivity with temperature in-the raftge of 18"C is reported to be 0.0216 % pet degree for chloride ions and 0.0227 % per degree for sulfate ions. 5.2 Filter Paper, conforming to Specification E 832, Tjpc 1, Class C, to keep silt from fouling the surfaces of ihe conductivity cell. 6. Reagents and Materials 6.1 Purity ofReagents--Reagent grade chemicals shall be used in till tests. Unless otherwise indicated, it is intended that all reagents conform to the specifications of the Com mittee on Analytical Reagents of the American Chemi'.il Society where such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 6.2 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type IV of Specification D 1193. 6.3 Potassium Chloride (KC1 or 0.02 N KC1 solution). 1 This specification is under thejurisdiction ofASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.46 on Industrial Protective Coatings. Current edition approved April 28, 1989. Published June 1989. 2 Annual Book ofASTM Standards, Vol 06.03 and 11.01 3 Annual Book ofASTM Standards, Vol 14.02 4 "Reagent Chemicals, American Chemical Society Specifications," Am Chemical Soc.t Washington, DC. For suggestions on the testing of reagents " I listed by the American Chemical Society, see "Reagent Chemicals and StandarL by Joseph Rosin, D. Van Nostrand Co., Tnc., New York, NY, and the "Uniicd States Pharmacopeia." 872 DU PO 502 98052 D 4940 Sampling 7.1 Sampling shall be as follows unless otherwise agreed upon between the purchaser and the seller. Take two 1-L ampies of abrasive at random from different packages of 'Uadi lot, batch, day's pack, or other unit of production in the |ipment. When no markings distinguishing between units if production appear, take samples from the different packages in the ratio of two samples for each 10 000 lb 000 kg), except that for shipments of less than 10 000 lb, |ake two samples. Test the samples separately. Calibration and Standardization Hj8.1 Determination ofCell Constant: 1 8.1.1 The conductivity cell will come with a predeter mined constant. This constant should be checked periodi cally, one method being as follows: 8.1.1.1 Prepare a standard solution such as a 0.0005 N fiilution of KCI by diluting a 0.02 N KC1 solution with water Ir by dissolving 0.0372 g of KCI (heated before weighing for 1% at 105C) in water, followed by dilution to 1 L. Cool and Seasure the conductance at 25C as described in Section 9. Calculate the cell constant, as follows: *25 = (cycj ^here: = conductance, measured at 25"C (see 10.1), pmho, and = conductivity, 72 pmho/cm (from Table 1). J|N' 3--In general the cell constant is not greatly affected by pHations in the strength of the KCI solution, but, for greater accuracy, jeasurements should be made at or near the specific conductivity ofthe Itotion to be measured and at values that utilize the middle range ofthe pale of the conductivity bridge, using tire same multiplier tap. 8.1.2 Table 1 gives values of specific conductivities for iSrresponding KCI solution concentrations which are useful pr abrasive testing. .Procedure . 9.1 Preparation ofa Slurry Filtrate: | 9.1.1 Rinse beakers, stirring rods, and funnels with rekent water until tests show the rinse water has a conduc|yity of 5.0 pmho/cm or less. Hi9.1.2 Add 300 mL of water to 300 mL ofabrasive and stir : 1 min with a stirring rod. Let stand for 8 min and then again for 1 min. u9.1.3 Filter sufficient supernatant liquid for tests, dis carding the first 10 mL of the filtrate. The amount of jrpernatant liquid filtered shall be sufficient to cover the cell. '9.1.4 Rinse the conductivity cell in reagent water until the pise water is a cleanliness of 5.0 pmho/cm or less. 1;9.1.5 Rinse the conductivity cell two or three times with he filtrate then determine conductance at 25C in accordfhee with the operating instructions of the instrument. Use successive portions of the sample until a constant value is obtained. 10. Calculation .10,1 Calculate the specific conductivity of the abrasive as follows: Cs -- C'm x 11. Report 11.1 Report the following information: 11.1.1 The calibration value of the cell constant (both as measured and as predetermined and supplied with the conductivity cell), the date, and the name of the person checking the calibration. 11.1.2 The material, date, readings and mean in jtmho/ cm along with name of person conducting the tests and identification of the apparatus. 12. Precision and Bias3 12.1 Precision--On the basis of five replicate interlaboratory tests of this test method in which three operators in three laboratories analyzed, in duplicate, six blasting abra sives containing ionogenic contamination, the within-laboratory coefficient ofvariation after rejecting results from one set of replicate tests as outliers, was found to be 1.7% with 20 degrees of freedom (df) and the between-laboratory standard deviation coefficient of variation was found to be 7.4 % with 15 df. Based on these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 12.1.1 Repeatability--Two results, each the mean of two runs obtained by the same operator should be considered suspect if they differ by more than 5 % relative. 12.1.2 Reproducibility--Two results, each the mean of two runs, obtained by operators in different laboratories should be considered suspect if they differ by more than 22 % relative. 12.2 Bias: 12.2.1 Bias can be present because of the mobility of various ions. The hydrogen ion has a much greater mobility than the hydroxyl ion or other ions so that at low pH's the conductivity will be relatively higher than at high pH's for the same ionic concentration. However, the bias introduced by this factor is in the proper direction. That is, high conductivity due to a lower pH of the contamination would normally indicate greater corrosion potential. 12.2.2 A bias may be introduced by extraneous contami nation or from reduced sensitivity of instruments for low levels of contamination in the range of conductivity between 0 and 30 jimho/cm. s TABLE 1 Specific Conductivities for Potassium Chloride (KCI) Concenirations at 25C H Normality Heated, Dry KCI/Reagent Water Solution, g/L KCI Conductivity, jimho/cm W 0.0005 K. 0.001 mk o,O05 W- '01 0.0373 0.0746 0.3728 0.7455 72 147 718 1414 13. Keywords 13.1 ionogenic; contamination; steel surfaces; abrasive; blasting; conductimetric; analysis; interlaboratory testing; precision; chloride; conductivity; salts. * Supporting data available from ASTM Headquarters. Request RR: DO 1-1061. 873 DUP050298053 # D 4940 The American Society tor Testing and Material? takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee andmust be reviewed every five years and Knot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the respons/b/e technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to tha ASTM Committee on Standards, ?9?6 ftece St., Pbtfadefphia, PA 79703. 874 DUP050298054 I Designation: D 4941 - 89 Standard Practice for Preparing Drawdowns of Artists' Paste Paints1 This standard is issued under the fixed designation D4941; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. I Scope 1.1 This practice covers the production of uniform films 'jartists' tube paints and other nonflowing pigmented paints ing paint applicators designed for less viscous paints. |i.2 Information on how to achieve opaque specimens these paints is included. .3 This standard may involve hazardous materials, oper- and equipment. This standard does not purport to s all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish mpriate safety and health practices and determine the Hcability ofregulatory limitations prior to use. Referenced Documents lt-?.l ASTM Standards: > "D 16 Terminology Relating to Paint, Varnish, Lacquer, - and Related Products2 4 4838 Test Method for Determining the Relative Tinting; . Strength of Chromatic Paints3 IB 1164 Practice for Obtaining SpectrophotometricxData for Object-Color Evaluation4 ' Terminology 1 3.1 Definitions'--See Definitions D 16 for definitions of terms used in this practice. 1 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 drawdown bar--a metal applicator with a specified sgap designed to deposit a wet paint film uniformly on a specified test panel (for example, an opacity chart) or other ' ubstrate. 3 2 2 drawdown--a layer of paint deposited op a substrate by se of a drawdown bar for the evaluation of paint characteristics. Summary of Practice 4.1 The paint is spread over the area ofthe test panel to be covered by the drawdown and the bar is pulled down with pressure just sufficient to avoid lifting of the bar from the chart surface. 4.2 Test panels are allowed to dry in a dust-free environ ment. 4.3 If complete hiding (opacity) is needed and not pro- duced by a single paint film, a second film is applied at a 90 1 Tliis specification is under the jurisdiction of ASTM Committee D-l on Paint nd Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.57 on Artist Paints and Related Materials Current edition approved April 28. 1989. Published June 1989. 2 Annual Book ofASTM Standards, Vols 06.01,06.02, and 06.03. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vol 14.02, angle to the first. If required, additional layers may be applied using a narrower drawdown bar. 5. Significance and Use 5.1 Quality standards for artists' paints require the evalu ation of various appearance characteristics of paint films. Tinting strength determination (Test Method D 4838) specif ically requires the preparation of drawdowns for colorimetric measurement. Other evaluations such as color designation, transparency, gloss, and color difference measurements also require drawdown samples. 5.2 Artists' tube paints have a paste consistency that makes the use of traditional film application methods difficult, especially for drying oil paints. 5.3 Artists' paints vary in two properties important to the preparation of films, that is, transparency and drying time. Colorimetric determination and some other types of evalua tion require paint specimens that completely hide the substrate. Very, transparent paints require such a thick film to produce complete hiding that drying times is excessively long or the specimen surface is blemished. When complete hiding is necessary, this practice is designed to provide opaque films without these defects through application of a series of thin film.. 6. Apparatus 6.1 Drawdown Bars, two, of different widths with a clear ance of 0.006 in. (0.152 mm). Recommended widths are 3 in. (7.6 cm) and 6 in. (15.2 cm). The second bar is required to prepare drawdowns with more than two layers. Wire wound drawdown bars have been found to be unsuitable.5 6.2 Drawdown Charts, sealed paper type, half black and half white if transparency is being evaluated or opacity is necessary.6 7. Procedure 7.1 Attach chart to a firm, smooth, level plane surface using tape, a vacuum plate, or a clamp. Label the chart with the identity of the specimen and other data as required. 7.2 Mix paint sample thoroughly using two spatulas. Tube paints that have separated should be expelled completely and mixed. N' 1--The use of coated freezer wrapping paper as a mixing surface simplifies clean up. The same paper can be used for weighing 5 Suitable drawdown bars can be obtained from the Paul N. Gardner Co., P.O. Box 10688, Pompano Beach, FL 33061-6688; or BYEC-Gardner, Inc., Gardner Laboratory, 2435 Linden Lane, Silver Spring, MD 20910. * Suitable charts can be obtained from The Leneta Co., Box 576, Ho-Ho-Kus, NJ 07423. 875 5 I *7 h- .f 9R ? DUP0502 98055 Drawdown Bar D 4941 Sealed Black & White Chart FIG. 1 Preparation for Drawdown specimens when required as in the tinting strength determination (Test Method D 4838). 7.3 Using a spatula, spread the paint, in a thickness exceeding the bar's gap clearance, over the entire area to be covered by the drawdown. Do not cover the area to be contacted by the supporting feet of the wider of the two bars. Starting at the top of the chart and using the wider bar, draw the bar down over the paint in an even rnotion applying sufficient pressure to ensure that the resistance of the viscous paint does not raise the feet of the bar from the surface. When using oil paints the motion should be slow enough to allow for the high viscosity. Acrylic paints, which have short drying times, should be applied immediately after mixing to avoid premature film formation. 7.4 After drying in a horizontal position for 15 min, specimens may be hung in a vertical position in a dust-free area to complete the drying. Allow 24 h for acrylic and alkyd paints and 48 h or longer for oil paints until dry to touch. 7.5 Examine the specimen for surface defects and discard if unacceptable. 7.6 If complete hiding is required, compare, either visu ally or instrumentally, the lightness of the paint on the black portion ofthe chart with that on the white. For instrumental evaluation, follow the procedures given in Practice E 1164 to determine CIE Y for each portion, then calculate the contrast ratio of the paint film on the two portions of the chart (CIE f|-.iack/CIE Fwhite). A .contrast ratio of 0.98 or higher is considered opaque. 7.6. t If opacity is not sufficient, rotate the chart through a FIG. 2 Three Overlapping Drawdowns 90 angle and deposit a second film using the wider bar to repeat the procedure' in 7.3 through 7.5. If additional layers i 11 are required, repeat this sequence using the narrower baf. lC careful each time that the feet of the drawdown bar ride on' the surface of the combined lower layers. See Figs. 1 and 2. , N' 2--The most transparent paints studied were found to require three coats; however, in some instances, such as with alizarin crimson >i paint, it may not be practical to obtain complete hiding. 77ie American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are express// advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn Yoor comments are invited either for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you fesi that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 876 DUPO 50298056 Designation: D 4942 - 89 Standard Test Methods for Water Pickup of Lithographic Printing Inks and Vehicles in a Laboratory Mixer1 This standard is issued under the fixed designation D 4942; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapprovol. A superscript epsilon le) indicates an editorial change since the last revision or reapproval. Scope ill These test methods cover two procedures for deterning the amount of water picked up by lithographic nting inks in a laboratory mixer. 1.2 Test Method A covers single-point water pickup; Test thod B covers the rate of water pickup. Both test methods applicable to any printing ink and vehicle intended for [lithographic printing process. .3 This standard may involve hazardous materials, oper;ns, and equipment. This standard does not purport to `dress all ofthe safety problems associated with its use. It is responsibility of the user of this standard to establish ropriate safety and health practices and determine the $j?licability ofregulatory limitations prior to use. ^Summary of Test Method '2.1 These test methods utilize a laboratory mixer for .ting water or other agreed upon fluid into the lest ink. 2 For single-point water pickup (Test Method A), 50 of water is normally added to 50 g of ink and mixed in ;r 5 min. The water picked up is determined from voluetric measurements of free water. 2.3 For rate of water pickup (Test Method B), water is dded to 50 g of ink in increments of 20 mL and mixed in 11 min or more over a cumulative time period totaUng 10 in. The water taken up by the ink after each mixing ierval is determined gravimetrically. Significance and Use 3.1 The lithographic printing process requires that some ampening solution be emulsified into the ink. These test -thods provide a rapid means for determining water ickup under laboratory conditions. Test results may be eful for specification acceptance between the supplier and ije customer. 3.2 In order that results be comparable, the tests must be :.n at the same temperature and with the same type and .iantity of liquid added prior to mixing. 3.3 The emulsions obtained in these test methods are of ger particle size than those typically produced in printing ps. Because of these and other variables in the printing rocess, water pickup results do not by themselves predict ithographic printing performance. ; 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint `M Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.56 on Printing.Inks. Current edition approved April 28, 1989. Published June 1989. 4. Apparatus 4.1 Laboratory Mixer,2 such as a Duke Ink-Water Emul sification Tester2 equipped with a stainless steel specimen bowl 83 mm wide and 88 mm high, mixer blades that rotate at 90 r/min, and a timing device. 4.2 Balance, accurate to 0.1 g, 600-g capacity, 4.3 Palette knives, two. 4.4 Thermometer, quick response. 4.5 pH Meter (optional). 4.6 Conductivity Meter (optional). 4.7 Graduated Cylinder, 50 Or 100-mL. 5. Reagents and Materials 5.1 Water--Deionized or distilled water, preferably having a pH of 5.0 to 7.0 (100 to 200 mL per sample); alternatively, fountain solution or other aqueous medium as agreed upon between the supplier and the customer may be used. 5.2 Cleanup Materials--Naptha and rags or tissues. 6. Test Specimen 6.1 A minimum of 100 g is sufficient for two determina tions. Before removing ink from the can, stir or otherwise ensure that the ink specimen is representative. Close the can and replace sealing tape immediately after each ink removal. 7. Conditioning 7.1 Condition the instrument, water, and ink samples in a constant temperature room or bath, preferably at 23 1C. 7.2 Prior to use, check the alignment of the mixer blades. With the power switch ofthe mixer in the off position, set the clean bowl into the turntable and engage the locking pin firmly into the slot in the side of the turntable. Tilt the mixer head back and insert the blades, marked left and right, into their respective holders.' Lower the mixer head. If the blades hit the side or bottom of the bowl, return the instrument to the manufacturer for realignment. 8. Test Method A--Single Point Water Pickup (by Vol umetry) 8.1 Program the counter of the mixer for 5 min mixing time (450 revolutions). 8.2 Optional--If the first run of the day, pour test water into a beaker. Measure pH, conductivity, and temperature at the beginning of testing. 8.3 Weigh or tare the clean dry mixing bowl. Add 50 2 Available from Duke Custom Systems, 8371 Highway 49, Pleasant View, TN 37146- 877 :] yi i m DUP050298057 # D 4942 0.1 g of the ink to the center of the bowl. 8.4 Pour 50 mL of water (from 8.2) into a graduated cylinder. If the ink is expected to pick up more than 100 % water, use 100 mL of water. Adjust the volume to 0.5 mL. Add the entire contents to the bowl. 8.5 With the mixer head tilted back insert the clean blades, marked left and right, into their respective holders. Lock the bowl on the turntable. Lower the mixer head. Press the counter reset button, making sure that 450 is displayed on the face of the counter. 8.6 Turn the mixer on. Examine contents of the bowl as mixing progresses. If 50 mL of water had been added and all of it disappears into the ink, stop, discard the ink in the bowl, clean up, and start over from 8.3, adding 100 mL ofwater in 8.4. The latter quantity must also be used for all other inks in the series under study. No t ' 1--With some inks, water pickup is affected by the amount of water added prior to mixing. When 50 mL is insufficient, do not simply add another 50 mL during the run, as test results may differ significantly from those obtained by adding LOO mL at the outset 8.7 When the mixer stops, turn the power switch off. Tilt the head out of the ink, detach the mixing blades, and add to the bowl. 8.8 Remove the bowl from the turntable and, holding the blades at the side of the bowl, decant the free water into a graduated cylinder. Run the blades very slowly through the ink in the bowl. Decant additional free water into.the cylinder. N' 2--Do not knock the bowl to force free water from the surface. Always handle the bowl gently to avoid breaking the emulsion. 8.9 Record the returned water level to 0.5 mL. 8.10 Optional--Measure the temperature, pH, and con ductivity of the returned water. Note the appearance of the water and the consistency of the ink arid the appearance of the returned water. 8.11 Discard ink left in the bowl. Clean the bowl arid the mixer blades with tissue wetted with naphtha. Discard the returned water and rinse the cylinder clean. 8.12 Repeat 8.3 through 8.10 with a second specimen of the same ink. 9. Test Method B--Rate of Water Pickup (by Gravimetry) 9.1 Program the counter for the first interval of the mixing cycle. N' 3--A commonly used cycle is 1-min intervals (90 revolutions) times ten determinations. Intervals need not be uniform, for example, 1, 2, 3, 5, and 10 min (90 times 3 plus 180 plus 450 revolutions). 9.2 Optional--Measure water properties in accordance with 8.2. 9.3 Weigh or tare the clean dry mixing bowl and blades on the balance. Add 50 0.1 g of ink to the center of the bowl. 9.4 Lock the bowl on the platform of the mixer. With the mixer head raised, carefully insert the blades into their respective holders. If ink on one blade touches the upper parts of the other blade or the side of the bowl, carefully remove the ink with two palette knives and transfer to the bottom of the bowl. Lower the mixer head. 9.5 Pour 100 mL of water (from 8.2) into a beaker. Meter out 20 mL and add to the bowl. 9.6 Press the counter reset button, making sure that the desired number of revolutions is displayed on the face of the counter. Turn the mixer on. Examine the contents of the ! '4$ bowl as mixing progresses. If all liquid disappears into the ''> ink, add more as needed to maintain a layer of excess water on the surface of the ink. N' 4--Few specimens will take up more than 20 mL of water within a 1-min mixing interval. If a high-water pickup specimen is being run and the mixing interval is longer than i min, another 20 mL should be added prior to each subsequent minute of mixing time. 9:7 When the mixer stops, turn the power switch off. Detach the mixing blades and add to the bowl. 9.8 Remove the bowl from the turntable and, holding the blades at the side of the bowl, decant the free water into the beaker containing the unused water. Run the blades very" slowly through the ink in the: bowl. Decant additional free water into the beaker (see Note 2). 9.9 Weigh the mixing bowl and contents, including thf blades. 9.10 Using a palette knife, transfer the ink from the walls to the center of the bowl. Return the bowl to the mixer Replace the blades as in 8.4. i; 9.11 For the next mixing interval, swirl the beaker in, order to mix the returned and unused water. Meter out 20 mL and add to the bowl. Press the counter reset (or change the counter) and turn the power on. Add more water i` needed to maintain an excess layer (see Note 4). 9.12 When the mixer stops, repeat 9.7 through 9.11 until the cumulative mixing time totals at least 10 min. 9.13 Optional--At the end of the run, make measure ments in accordance with 8.10. 9.14 Discard the ink left in the bowl. Clean the bowl and the mixer blades with tissue wetted with naphtha. Discard returned water and rinse the beaker dean. 9.15 Repeat 9.3 through 9.14 with another specimen cf the same ink. 10. Calculation 10.1 Calculate water pickup, P, as follows: 10.1.1 Test Method A--Volumetric: /> = ((/,- F2) x 2 where: P = water pickup, % or mL water/100 g ink, K, = volume of water added, mL, and V2 = volume of returned water, mL. 10.1.2 Test Method B--Gravimetric: p = (W-S)x. 2 where: P = water pickup, % or g water/100 g ink, W - weight of the specimen plus water picked up after each .mixing interval, g, and 5 = weight of initial specimen, g. N' 5--The conversion from water pickup of the ink to water content, C, of the emulsion is C = P/(l00 + P). Units are percent or grams of water per 100 grams of emulsion. 11. Report 11.1 Report the following information: 11.1.1 The percent water pickup to the nearest whole number as the mean of the two determinations, the cumula tive mixing time, and a description of the water used for 878 DU PO50298058 ft D 4942 posting (for example, tap water, deionized water, or type of fountain solution). 11.1.2 If rate of water pickup was determined, plot the percent of water pickup versus the cumulative mixing time. 11.1.3 Optional--The mean temperature, changes in pH, onductivity, appearance of the water, and the change in lonsistency of the ink. |pZ. Precision and Bias 12.1 Precision: H 12.1.1 Test Method A--An interlaboratory study of sin gle-point water pickup by Test Method A was conducted in ^yhich one operator in each of eleven laboratories tested in ^duplicate on each oftwo days three litiiographic printing inks igpging in 5-min water pickup from 50. to 65 %. One Company was found to be an outlier and was deleted from he analysis. The within laboratory pooled standard deviajfibn was found to be 1.58 % absolute (millilitre of water per 00 grams of ink) at 9 degrees of freedom (df), and the jfetween laboratories pooled standard deviation was 7.1 % psolute at 30 df. Based on these standard deviations, the pillowing criteria should be used forjudging the acceptability If results at the 95 % confidence level: r 12,1.1.1 Repeatability--Two results, each the mean of Bvo runs obtained by , one operator, should .be considered fgspect if they differ by more, than 4.5 % absolute. 12.1.1.2 Reproducibility--Two results, each the mean of jjsvo runs obtained by operators in different laboratories, pshould be considered suspect if they differ by more than |0 % absolute. 12.1.2 Test Method B--In an irtterlaboratory study' of rate of water pickup by Test Method B, water pickup values at 2'h, 5,1'h and 10 min were determined twice on one day by one operator in each of nine laboratories on six inks. The inks ranged in water pickup from 40 to 52 % at 2`A min and from 65 to 100 % at 10 min. After rejecting 12 out of 156 replicated test values as outliers, the within laboratory pooled standard deviation was found to be 1.58 % absolute (grams of water per 100 grams ink) with 97 df and the between laboratory standard deviation 3.73 % absolute with 86 df. Based on these standard deviations, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 12.1.2.1 Repeatability--Repeatability cannot be deter mined as both runs were conducted on the same day. 12.1.2.2 Reproducibility--Two water pickup curves, each the mean of two ruris, obtained by operators in different laboratories should be considered suspect if they differ by more than 10.5 % absolute. 12.2 Bias--Bias cannot be determined because there are no standard materials. The poorer interlaboratory precision of Test Method A compared to Test Method B is believed to be caused by the faet that the gross quantity of water added at one time is picked up as large globules which make it difficult for different operators to release free water in the same manner: 13; Keywords 13.1 lithographic printing inks; printing inks; inks; vehi-' cles; water pickup; water content; emulsification; fountain solution; mixers 7he American Society tor Testing and Materials takes no position respecting t/te validity of any patent rights asserted in connection . with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity ot any such patent rights, and the risk of infringement of such, rights, are entirety their own responsibility. This standard is subject to revision at any time, by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Raca St., Philadelphia, PA 19103. 879 DUP0502 98059 < Designation: D 4946 - 89'ei Standard Test Method for Blocking Resistance of Architectural Paints1 This standard is issued under the fixed designation D 4946; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reappraval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. ** N' --Paragraphs 6.5, 7.2, and 7.5 were editorially corrected in October 1990. 1. Scope 1.1 This test method describes an accelerated procedure for evaluating the face-to-face blocking resistance of trades sales paints. This is not to be confused with blocking resistance Test Method D 3003 which is concerned with blocking of industrial coatings on metal substrates, nor with Test Method D 2793 which is concerned specifically with wood product finishes and reports results on a satisfactory or not satisfactory basis, rather than by the degree of blocking tendency as in this test method. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safetyproblems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 2793 Test Method for Blocking Resistance of Organic Coatings on Wood Substrates2 D 3003 Test Method for Pressure Mottling and Blocking Resistance of Organic Coatings on Metal Substrates2 3. Terminology 3.1 Definition: 3.1.1 blocking--The undesirable sticking together of two painted surfaces when pressed together or placed in contact with each other for an extended period of time. 4. Summary of Test Method 4.1 Dried paint films are placed face-to-face and a pres sure of about 1.8 psi (127 g/cm2) is applied. These paint films are put into an oven for 30 min to make the test more stringent. After cooling, the blocked panels are peeled apart. The degree of blocking is rated subjectively for tack or seal using a series of standard descriptive terms corresponding to numerical ASTM values of 10 to 0. 5. Significance and Use 5.1 Dry paint often comes in contact with itself especially in window and door areas and, depending on its hardness, 1 This \es\ meihod is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D0I.42 on Architectural Finishes. Current edition approved May 26, 1989. Published July 1989. 3 Annual Book ofASTM Standards, Vol 06.01. the pressure, temperature, humidity, and duration of time the surfaces are in contact, sometimes sticks to itself (blocks). This stringent test method can be used to compare and iate subjectively the resistance of paints to blocking. 6. Apparatus 6.1 Conditioned Room, at 65 to 85"F (18 to 29.5C) and 40 to 60 % relative humidity. 6.2 Sealed Paper Test Charts, approximately 7.5 by 11 in, (190 by 280 mm).3 6.3 Applicator Blade, 5 to 6 in. (13 to 15 cm) wide, 6 mil clearance. 6.4 Oven, 1 f 5 to 125F (48 to 52C). 6.5 Rubber Stoppers, No. 8, 1.25 in. (3.2 cm) smallc, diameter. 6.6 Weights, 1000 g. 6.7 Scissors. 6.8 Aluminum Tray or Pan, flat. 7. Procedure 7.1 Cast the paint to be tested on a sealed test chart using the applicator blade. Condition coated panels in the condi tioned room for seven days. All painted panels should be kept free of grease, oil, or fingerprints since these will affect block resistance. 7.2 After the panels have been conditioned, cut out six t`/2 by l'/2-in. (3.8 by 3.8-cm) sections from the paintrv chart. Start the cut at least 'h in. (1.3 cm) away from the edge of the drawdown. 7.3 Place the cut sections with the paint surfaces fac.to-face for each paint to be tested. 7.4 The weights, stoppers, and tray should be temperatureequilibrated in the oven prior to running the test. 7.5 Place the face-to-face specimens in the oven on a flei aluminum tray. Place a No. 8 stopper on top, with the small diameter incontact with the specimens, then place a 1000-g weight on top of the stopper. This results in a pressure of 1 > psi (127 g/cm) on the specimens. One weight and stopper is to be used for each specimen to be tested. It is recommended that "pass" and "fail" paint controls be used in each test run and that the tests be run in triplicate. 7.6 After exactly 30 min, take the stoppers and weights off the test specimens and remove them from the oven. Aliev them to cool for 'h h in the conditioned room before determining the block resistance. 'Form WB available from The Leneta Co., P.O. Box 86, Ho-Ho-Kus. '1 07423 has been found satisfactory for this purpose. 880 DUP05 02 98060 # D 4946 7.7 After cooling, separate the specimens by peeling them apart with a slow and steady force at about 180 from each p other forming a UT" pattern during beginning of the separation. It is necessary to put the specimen next to the ear while separating to actually hear the degree of tack. Rate for flocking resistance on a scale of 0 to 10 (see 8.2). 8. Interpretation of Results 8.1 Blocking resistance is rated on a scale of 10 to 0, . which corresponds to a subjective tack (sound of separation vhen peeled) or seal (the* complete sticking together) rating determined by the operator. This rating system is defined in '.2 in the appropriate descriptive terms. The degree of seal is |the estimated area on the specimens where the paint surfaces here and some of the paper tears away From the chart . when peeled. 8.2 Blocking Resistance Ratings: Blocking Resistance iNumerical Ratings 10 9 8 Type of Separation no tack trace tack very slight lack Performance perfect excellent very good Blocking Resistance Numerical Ratings Type of Separation Performance very slight to slight tack slight tack moderate tack very tacky; no seal 5 to 25 % seal 25 to 50 % seal 50 to 75 % seal 75 to 100 % seal good to very good good fair poor to fair poor poor very poor very poor 9. Report 9.1 Report the blocking resistance rating determined in accordance with 8.2. 10. Precision 10.1 Data are unavailable for a conventional precision statement. However, based on actual laboratory experience, with experienced operators, the repeatability is estimated to be plus or minus one blocking resistance unit. Numerical values may differ from operator to operator but relative ranking should be about the same. As in many tests the precision improves with practice. 11. Keywords 11.1 blocking; blocking resistance; sticking; tack The American Society for Testing and Materials takes no position respecting the validity ot any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination ot the validity of any such patent rights, and tha risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or toradditional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 881 DUPO 502 98061 Designation: D 4948 - 89 Standard Test Method for Determination of the Upper Layer Separated from a Viscous Liquid1 This standard is issued under the fixed designation D 4948; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (<> indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the amount of liquid separated as an upper layer in a 24-h period from viscous solutions or dispersions that contain dispersed solids such as paints, enamels, pigmented lacquers, adhe sives, polishes, and other similar materials. N' --The amount of clear liquid that separates during this test is one of the criteria in the United Nations Recommendations on the Transportation of Dangerous Godds2 for the placement of flammable viscous liquids into packing groups related to flash points (See 4.1). 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standard: D 3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings3 3. Summary of Test Method 3.1 A measured amount of the material to be tested is placed in a graduated cylinder and allowed to stand undis turbed for 24 h. The volume percent of the separated top layer is then determined. 4. Significance and Use 4.1 The United Nations Committee of Experts on the Transport of Dangerous Goods in their recommended regu lations place materials having a flash point below 73.5F (23C) in Packing Group II. However, if viscous substances such as paint and related coatings, adhesives, polishes, etc., meet certain requirements, they can be placed in Group III along with materials having a flash point between 73.5 and 140T (23 and 60.5C). One of the requirements is that less than 3 % of clear liquid separates from the bulk of the material when subjected to this test method. 4.2 At the present time most international regulatory bodies such as the International Civil Aviation Organization 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.22 on Health and Safety. Current edition approved May 26, 1989. Published July 1989. 2 Transport of Dangerous Goods: Recommendations of the Committee of Experts on ii\e Transport ofDangerous Goods, United Nations; 3rd cd.. New York, 1984. 3 Annual Book ofASTM Standards, Vol 06.01. (ICAO) and the International Maritime Organization (IMO) j use the U.N. Recommendations. It is anticipated that most national transportation regulatory bodies will adopt the U.N,: Recommendations as their regulations for control of trans-! portation of hazardous materials. At present the United j States permits the transshipment of hazardous materials: through the United States to other countries, under regula-; tions of the IMO and ICAO. 5. Apparatus 5.1 Graduated Cylinder,4 100-mL, glass-stoppered, 250- mm total height and 30-mm inside diameter. 5.2 Constant Temperature Cabinet or Room, at 73.5 + 3.5F (23 2C). 6. Sampling 6.1 Obtain a uniform quart sample of the material using j standard methods for sampling in accordance with Practice S D 3925. 7. Conditioning 7.1 Store the sample or a representative portion at a ^ constant temperature of 73.5 3.5F (23 2C) until the ] sample reaches a uniform temperature of 73.5F (23C). 8. Procedure 8.1 Thoroughly stir the sample to obtain uniform con-Jf sistency and, in the case of materials containing particles, uniform dispersion of these particles. 8.2 Immediately pour 100 mL of the sample into the graduated cylinder. Insert a stopper and leave the cylinder'] undisturbed at 73.5 3.5F (23C) for 24 h. j 8.3 After 24 h, measure the volume of any upper sepa rated layer and determine the percent of the separated layer|j compared to the total volume of the specimen. 9. Calculation 9.1 Calculate the volume percent of the clear upper liquid !j layer Pc as follows: PC=(VJVJ x 100 where: Vc = volume of the clear upper liquid layer, mL, and Vm = total volume of the 100-mL specimen, mL. 4 A graduated cylinder. Catalog No. 2982-100, available from Coming Glass ; Works, Coming, NY 14831, has been found satisfactory for this purpose. 882 DU P050298062 D 4948 llO. Report f; 10.1 Report the volume percent of the separated clear [iiiquid to within 0.5 %. .11 Precision and Bias 11.1 The precision of this test method will be determined. 11.2 Bias cannot be determined since no standards are available. The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility, This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend; If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 883 DUP050298063 Designation: D 4958 - 91 Standard Test Method for Comparison of the Brush Drag of Latex Paints1 This standard is issued under the fixed designation D 4958; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision, A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method is a standardized brushout procedure for comparing the brush drag of architectural type latex paints. 1.2 With slight modifications this test method is also applicable to solvent paints. 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user ofthis standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 1475 Test Method for Density of Paint, Varnish, Lac quer and Related Materials2 D 3924 Specification for Standard Environment for Con ditioning and Testing Paint, Varnish, Lacquer and Related Materials2 D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 D4287 Test Method for High-Shear Viscosity Using the ICI Cone/Plate Viscometer2 3. Terminology 3.1 Definitions--See Paint/Coatings Dictionary3 for defi nition of terms used in this test method. 3.1.1 brush-drag-- resistance encountered when applying a coating by brush. 4. Summary of Test Method 4.1 A 2-in. (50-mm) polyester brush is used to apply the test paint on a 1.076-ft2 (1000-cm2) test area. The applica tion is made at a spreading rate of 400 ft2/gal (9.82 m2/L) and is completed in 30 to 35 s. The degree of brush drag is rated subjectively using a series of standard descriptive terms corresponding to numerical values of 1 to 10. The rank order of a set of samples is thereby established. 5. Significance and Use 5.1 As the brush drag of a paint increases, any natural tendency on the part of the painter to overspread the paint is 1 This lest method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee DO 1.42 on Architectural Finishes. Current edition approved Oct. J5, 1991. Published December L99I. Originally published as D 4958 - 89. Last previous edition D 4958 - 89. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Available from Federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. reduced. When all other factors are held constant, increased brush drag will result in greater film thickness with conse quent improvement in durability and hiding. Conversely, sometimes it might be preferred to have a lesser degree of brush drag for easier application (that is, the amount of time and effort in applying a paint to a specific area is reduced with a lesser degree of brush drag). 5.2 This test method provides a standardized brushout procedure for the evaluation of brush drag as an alternative to customary informal ad hoc procedures. Its objective is to maximize the reliability and precision with which this characteristic may be determined. N' 1--The brush drag of paints is directly related to their, high-shear viscosity. There is generally good rank order agreement between results obtained by this method and Test Method D 4287. Thei sensitivity of this brushout method has been found sufficient to distinguish between brushabilities corresponding to high-shear viscosity differences not lower than 0.3 poise (0.03 Pa.s). Round robin data show that rank order agreement between the brushout and viscometric methods is poor when latex and solvent paints are part of the same comparison group. This is the result of these two paint types having markedly different rheological properties that affect the relative percep tion of brush drag.'4 ,6. Apparatus 6.1 Brush, 2-in. (50-mm) polyester filament, 2Va-in. (70mm) length-out, Vie in. (14 mm) thick, with a chiseled tip. : N' 2--All tests of a given series of paints, within or between i laboratories, should be carried out with commercially identical brushes. 6.2 Stopwatch. 6.3 Balance, capable of weighing accurately to 0.1 g. 6.4 Test charts, with a sealed surface, having 1.076 ft2 f (1000 cm2) of test area.5 7. Sampling and Conditioning 7.1 Sample in accordance with Practice D 3925. 7.2 Condition the samples in accordance with the Condi-i, tioning and Testing section of Specification D 3924. 7.3 All testing should be performed under the same conditions. 8. Procedure 8.1 Do not change operators during the running ofa series of specimens, since this will invalidate any conclusions as to rank order. 8.2 Determine the density in pounds per gallon of the paint sample in accordance with Test Method D 1475. "Supoporting data are available from ASTM Headquarters. Request RR: D01-1072. 5 Lencta Form 8H-BW. obtainable from The Leneta Co., P.O, Box 86, Ho-Ho-K-tis, NJ 07423, has been found satisfactory for this purpose. 884 DUP0502 98064 D 4958 |S.3 Multiply the density by 1.221 to obtain the weight of c in grams to apply on the specified test chart to obtain a ading rate of 400 ft2/gal (9.82 m2/L). it8.4 Conditioning ofthe Brush: 8.4.1 Soak the brush in clean water, then spin rapidly to nove the water from the bristles as completely as possible. |!78.4.2 In order to equalize the amount of paint contained i the brush, dip the brush into the can to take up a normal i load and paint out approximately `/z ft2 (0.05 m2) of a onably well sealed surface (for example, any previously nted test chart). 1.4.3 Repeat 8.4.2 utilizing another dry surface. Place the test chart on the balance and weigh the t amount of paint as calculated in 8.3 directly onto the er of the card. Immediately tape the card onto a hard, flat surface, t the stopwatch, and proceed to spread the paint using the eviously conditioned 2-in. (50-mm) brush. Using long, ady brush strokes, alternately parallel and perpendicular f the edge of the chart, cover the test area uniformly and Ompletely in 30 to 35 s. i8.7 Immediately assign and record a brush drag rating ccording to the following series of qualitative descriptive ns, first characterizing it by a verbal description, and then ; corresponding number. 1--Very slight ' 2--Slight 3--Slight to moderate 4--Moderate 5--Moderate to considerable 6--Considerable '17--Considerable to pronounced 8--Pronounced 9-- Very pronounced ' 10--Extreme : 8.8 Thoroughly clean the brush with warm water and spin to remove excess water between tests. 8.9Repeat 8.2 through 8.8 for each specimen in the set and rate the specimen as the mean of the two results. 8.10 If more than one specimen has the same rating, brush out the similarly rated specimens again, in close comparison. If small differences are perceived, then indicate these by assigning intermediate decimal values. If no differ ence is found then the original ratings stand. 9. Interpretation of Results 9.1 Tabulate the paints in order of their brush drag ratings, showing verbal descriptions and numerical ratings in separate columns. 9.2 In a fourth rank order column, rank the paints from 1 to n (least to most brush drag), where n is the total number of paints in the series. 9.3 Paints with the same qualitative ratings should be assigned multiple rank numbers, with the mean of those numbers shown in parentheses, for example, 3 to 4 (3.5), 5 to 7 (6). The mean ranking value (in parentheses) is used to calculate an average ranking value when the same series of paints is ranked by more than one operator. 10. Report 10.1 Report the brush drag ranking as determined in Section 9. 11. Precision and Bias 11.1 In an interlaboratory study of this test method in which five coatings varying widely in brush drag were ranked by one operator in each of nine laboratories, two operators in one laboratory, and three operators in another, laboratory, the coefficient of concordance (agreement in ranking) was found to be 0.84, reflecting the fact that seven ofthe fourteen operators agreed perfectly and four others reversed one of two adjacent pairs. The coefficient is statistically significant at the 99.9 % confidence level. 11.2 Bias has not been determined for this test method. 12. Keywords 12.1 brush drag; high shear viscosity; brushabiiity; ease of brushing; drag The American Society tor Testing and Materials takes no position respecting the validity of any patent rights assertedIn connection with any item mentioned tn this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feei that your comments have not received a fair hearing you should make your views known to (he ASTM Committee oh Standards, 1916 Race St., Philadelphia, PA 19103. 885 fed DUPO 502 98065 i Designation: D 4960 - 89 Standard Test Method for Evaluation of Color for Thermoplastic Traffic Marking Materials1 1 m , ''tluin fon i This standard is issued under the fixed designation D 4960; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision, A number in parentheses indicates the year of last reapproval A superscript epsilon (t) indicates an editorial change since the last revision orreapproval. X. Scope 1.1 This test method covers the instrumental determina tion of color of thermoplastic traffic marking materials in the CIE 1931 system, 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory Imitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D883 Definitions of Terms Relating to Plastics12 E 97 Test Method for Directional Reflectance Factor, 45-Deg 0-Deg, of Opaque Specimens by Broad-Band Filter Reflectometry3 E 179 Practice for Selection of Geometric Conditions for Measurement of Reflectance and Transmission Proper ties of Materials4 E 284Terminology Relating to Appearance of Materials4 E 308 Test Method for Computing the Colors of Objects by Using the CIE System4 E 1164 Practice for Obtaining Spectrophotometric Data for Object-Color Evaluation4 F 412 Definitions of Terms Relating to Plastic Piping Systems5 3. Terminology 3.1 Definitions--Definitions are in accordance with Defi nitions D 883, E 284 and F 412, unless otherwise indicated. 3.2 Descriptions of Terms Specific, to This Standard: 3.2.1 thermochromism--a color hue change that takes place in the thermoplastic material due to temperature changes. 3.2.2 thermoplastic traffic marking material--a highly filled 100 % total solids highway marking material that when heated to a molten state can be extruded or sprayed onto a road surface and when cooled forms a solid, durable delin eator. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is under the direct responsibility of Subcommittee DO 1.44 on. Traffic Coatings. Current edition approved June 30. 1989. Published August 1989. 2 Annual Book ofASTM Standards, Vol 08.01. 2 Annual Book ofASTM Standards, Vols 06.01 and 14,02. 4 Annual Book ofASTM Standards, Vol 14.02. 5 Annual Book ofASTM Standards, Vol 08.04. 4. Summary of Test Method 4.1 The thermoplastic specimen is prepared for this test by melting a sample to its application temperature under continuous agitation and then pouring it' into a TFEfluorocarbon coated pah, to form a patty of approximately 3 in. (7.6 cm) in diameter. The patty is allowed to cool to room temperature before measuring the color. Color measure ments are made on the flat side or the top side of tU thermoplastic patty. s,Auft1 if noo N' 1--No significant color differences are encountered in reading the top or bottom of the patty. 5. Significance and Use 5.1 This test method provides a standard procedure foi the determination of color of thermoplastic traffic marking materials. This test method can be used in conjunction with specifications to determine the uniformity of thermoplastic traffic marking materials from batch to batch and that produced by various suppliers. 5.2 There is a slight variation in color standards and colorimeters. This test method is only applicable when results are reported with the instrument model'designation and white color calibration standard identification informa tion. 6. Sampling 6.1 Samples may be obtained by an appropriate quar-, tering or riffle sampling method where deemed necessary considering the physical form of the material. 7. Apparatus 7.1 Agitator Blade, 6 in. (15 cm) long with a Vi-in. (1 -cm) steel shaft and a PA by I by Vs-iti. (4.5 by 2.5 by 0.3-em)' straight horizontal steel blade. 7.2 Drill Press, or other apparatus capable of agitating the thermoplastic marking material in the electric pots at 600 to 700 r/min during meltdown to the application temperature 7.3 Heating Equipment: 7.3.1 Gravity Convection Oven, capable of maintaining 260C, for melting the thermoplastic traffic marking. 7.3.2 Hot Plate, capable of maintaining 537<'C. 7.3.3 Insulated Electric Pots, for heating and melting the thermoplastic traffic marking materials. 7.4 Color Measuring Instrument, conforming to all re quirements of Test Method E 97, Practices E 179 and E 1164, and Method E 308 (geometry 45/0'\ illuminanl (, 2 observer). 7.5 Spatulas, for stirring the thermoplastic traffic marking 886 DUP050298066 D 4960 Bring meltdown on the hot plate or in the gravity convec- on oven. 7.6TFE-fluorocarbon Baking Pans or Uncoaied Pint Can Uds, for forming 3-in. (7.6-cm) diameter patties. -8. Procedure 8.1 Taking care to prevent scorching of the material, melt :k ,1000 50-g sample of the thermoplastic marking material i'tTa temperature of 2I8C under continuous agitation, by !i e of the following means: 8.1.1 On a. hot plate set at 537C and using a spatula as means of agitation. , i-:;8.1.2 In an insulated electric pot with a heat setting (ficient to reach the test temperature and with agitation of 0 to 700 r/min from an electric drill press or other suitable eans. : - 8,1.3 In an oven set at 260C with agitation by stirring th a spatula after thefirst 15 min and thereafter at 15-riiin tervals. The first stirring at 15 min is critical to' prevent rehing of the thermoplastic marking material. The sample ust be completely wet in on the first stir to ensure even elting and complete blending of the components of the rmoplastic material. 8.2 Pour the thermoplastic sample into a clean, T&& orocarbon-lined pan, to form a 3-in. (7.6-cm) diameter tty. If a TFE-fluorocarbon pan is not available, pour the mple into an uncoated pint tin lid to form a 3-in. diameter tty. Before pouring the patty, the sample must be agitated 11 to prevent settling of the components and to providea smooth homogeneous surface for color measurement. 8.3 Allow the patty to cool to room temperature for a " inimum of 30 min and not to exceed 45 min. No t ' 2--A 30 5-min conditioning of the patty negates the initial effects of thermochromism. 8.4 Calibrate the,color measuring instrument with a white calibration color standard according to the instructions supplied by the manufacturer. 8.5 Remove the patty from the TFE-fluorocarbon pan and read the color measurement values from the flat smooth side. If a pint tin lid is used then read the top of the patty. Without removing the patty from the sample port immedi ately take three readings. Record only the third reading for each y, x, and y value to further compensate for any thermochromism of the thermoplastic marking material. 8.6 A small port adapter,, if available,, for, the color measuring instrument of approximately% in. (19 mm), may be used to negate the effects of,geometry and texture when reading the patties. This will measure, in between small surface imperfections, characteristic of thermoplastic traffic marking. ,, 9. Report 9.1 Report the following information:. 9.1.1 The formula code,' batbh number, formula type, and color for each patty read,' 9.1.2 The type of color measuring instrument used and the identification of the white color calibration standard, and 9.1.3 The exact cooling period and values- F, x arid y for each sample. 10. Precision and ljias 10.1 No general statement of precision can hei made because of lack of sufficient data at this time.: 10.2 No statement of bias can be prepared for this test method since there is no absolute test method for use as a comparative basis. 11. Keywords' ' 11.1. thermoplastic traffic marking; color measurement. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination ofthe validity of any such patent rights, and the risk ot infringement ofsuch rights'; are entirely {heir own respPhsfbllHy/ tJ This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not, revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you imy attend. If you fee/ that ydur comments have not received a fair hearing you sftou/d make your vf&NSknowntothe ASTM Committee bn Standards, 191$ Hade St., Philadelphia, PA 19103. ' - 887 DUP050298067 Designation: D 5007 - 89 Standard Test Method for Wet-to-Dry Hiding Change1 This standard is issued under the fixed designation D 5007; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an, editorial change since the last revision or reapproval. 1. Scope to give a standard degree of contrast just short of complete 1.1 This test method covers the determination of the hiding. change in hiding power of an architectural coating during 3.1.2.1 Discussion--In reflectometry the standard con drying, by visual evaluation of the wet and dry film. trast for hiding power measurements is generally accepted 1.2 This test method is not recommended for colors other the contrast ratio C = 0.98, which with white and light tinted than white and tints. coatings is equivalent to a visual color difference of about 1.3 This standard may involve hazardous materials, oper 0.75 CIELAB units. That amount of color difference can ations, and equipment. This standard does not purport to reasonably be described as "just-short-of complete-hiding " address all ofthe safety problems associated with its use. It is Since this is a visual method it employs a visual comparator the responsibility of the user of this standard to establish as a standard, which is a hiding power chart with a white appropriate safety and health practices and determine the coating applied at a contrast ratio of 0.98. applicability ofregulatory limitations prior to use. 3.1.3 logicator--a multi-notch applicator with clearances, 2. Referenced Documents and corresponding wet film thicknesses and spreading rales, in equal percentage steps. 2.1 ASTM Standards: D2805 Test Method for Hiding Power of Paints by Reflectometry2 D 3924 Specification for Standard Environment for Con ditioning. and Testing Paint, Varnish, Lacquer, and Related Materials2 3.1.4 logicator scale--a scale whose values are in dirru. linear relationship with the logarithms of corresponding spreading rates. A specified change in scale value represents the same percentage change in spreading rate over any part of such a scale. 3.1.5 spreading index, h--the spreading rate expressed in logicator scale units (LU) as described in 3.1.4 and 4.1.". 3. Terminology 3.1.6 spreading rate, H--the area covered per unitq' .ra 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 hiding index, hs--the Spreading Index at a standard film opacity. In this test method the latter is a visual contrast standard prepared by applying a semi-opaque white coating rity of coating. (In this test method the quantity is volu metric). 3.1.7 TG19 logicator--a logicator designed for this lest method with eight notches numbered at four-unit intervals on a black and white hiding-power chart to give a contrast on a scale from 20 to 48, the notch clearances ranging from ratio of0.98 which isjust short ofcomplete hiding, and is the 2.65 to 10.4 mils {67 to 264 pm) corresponding to wet film conventional so-called full hiding end point in photometric thicknesses from 1.46 to 5.7 mils (37 to 145 pm) and hiding-power methods such as Test Method D 2805. Refer to spreading rates from 280 to 1100 ft2/gal (6.9 to 27 my LI, the hiding indices of the wet and dry films as hSVJ and ftSD with one scale unit representing, a change of 5 % and the respectively. four-unit interval between notches a cumulative change of 3.1.1.1 Discussion--Since this test method is intended to 21.55 % in the clearance and. corresponding film thicknesses measure hiding-power difference rather than hiding power and spreading rates. Refer to this scale unit as a logicator ur t itself, a 98 % contrast ratio standard is not required. It is (LU). (See Fig. 1.) necessary only that the same standard be used for measuring both wet and dry films. See 3.1.8.1. For this purpose the 3.1.7.1 Discussion--The percentage difference between notches is calculated as (1.054 -- I) x 100 = 21.55. i Ins standard needs to lie within the contrast range of both the percentage is applicable precisely to the notch clearances and wet and dry stripes, which will be true of the 98 % contrast- approximately to their related wet-film thicknesses and ratio standard for most commercial paints. With paints of spreading rates. The detailed relationships between scalar unusually low hiding, a lower contrast standard may be value and the notch clearance, wet film thickness, and required, which can be simply one ofthe stripes taken from a spreading rate are given in Tables 1 and 2. drawdown of the test paint. 3.1.8 wet-to-dry hiding change (WDHC)--the difference 3.1.2 hiding power--the spreading rate of a paint applied in the Hiding Index of a paint between the wet and the dry uniformly on a standard black and white hiding power chart ' state, expressed in logicator units (LU) as follows; WDHC -- tshs -- hSD -- hsw 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.42 on Architectural Finishes. Current edition approved October 27, 1989. Published December 1989. 2 Annual Book ofASTM Standards, Vol 06.01. 3.1.8.1 Discussion--The WDHC is unchanged if the con trast level of the hiding standard is varied, because the resultant changes in the two hiding power values will be proportional and their ratio therefore constant. 888 Sapps 4&WK 6t urav DUP050298068 D 5007 --t* *-0 1 A =0.70 inches (I7.emrn) 8 - 0.057 inches (1.45 mm) C " 6 inches {1S2.5 mm) 6 * 0.25inches (6.35 mm) E - 0.125 inches (3.18 mm) -ife ^\i TGI9 'U=N<=rA 28 40 k' JG mils' urn 20 10.40 264 24 8.S6 217 20 7.04 173 h mils* pm 32 5.79 147 36 4.76 121 40 3.92 100 44 3.23 82 48* Ti2rg.6ci5Vshoe67 FIG. 1 Diagram of the Leneta TG19 Logicator ^1,1.8.2 Discussion--The WDHC is unaffected by deviajdps from the estimated film thickness/clearance ratio T/N sp Note, Table I), because the ratio of the two recalculated ding-power values is unchanged. fJjSummary of Test Method gj.l The test paint is applied with a TGI9 Logicator on a Scator test chart (see 6.2 and Fig. 2) and the drawdown Imined in comparison with an agreed hiding standard ^mediately after application and again after drying. 4,2 The scale numbers of the wet and dry stripes that ^tch the standard in contrast are recorded as the Wet ding Index, hsW, and the Dry Hiding Index hSD. if3 The difference between the wet and dry hiding indices corded as the wet-to-dry hiding-change WDHC. 4.4 If desired, the percent change in hiding power correp'otiding to the WDHC value is calculated and reported; I' Significance and Use 5-.1 Many architectural paints, particularly white and light fits, change significantly in film opacity as they dry. An crease in hiding is sometimes associated with porosity and eor film integrity with conventionally formulated coatings, decrease can result in a disappointing paint job. The Bt-to-dry hiding change is therefore a property of great (radical importance. ?5.2 This test method can be used in paint specifications Bid as a short, simple procedure for evaluation and quality patrol. Apparatus tei 6.1 TG19 Logicator3--A multi-notch, variedtolearance jpplicator designed specifically for this test method (see 3.1,7 ud Fig. 1). 1)6.2 Logicator Test Charts3--Black and white hiding parts with a chevron-stripe pattern and scale numbers Jrinted at the top corresponding to the paint stripes applied Jy the Logicator (see Fig. 2). if6.3 Vacuum Plate, for holding the chart flat while the drawdown is made. j: 6.4 Visual Hiding Standard4--A narrow stripe cut from a ||gicator test chart on which a durable glossy white coating jf|(ad been applied to obtain a contrast ratio of0.98. The stripe TABLE 1 Equations Relating the Logicator Scale Value or Spreading Index, h, to the Notch Clearance, N, Wet Film Thickness, T, and Spreading Rate, H N' --The relationships Involving T and H are based on a presumed T/N ratio of 0.55, which ratio is approximate and somewhat variable, depending on coating rheology, drawdown technique, and clearance. Inch-Pound Units (mils, ft2/gal): Metric Units (nm, rr^/L): ' N = 1.056s'h - 27.6 + 1.05h h = 68 - 47.2 Jog N 0.65 N = 15.18-1-1.05'' h 55.75 - 47.2 log T H = 105.7 X 1.05" h * 47.2 log H - 95.52 N = 26.4 x 1.05s8-'' = 701 + 1.05'' h = 134.3 - 47.2 10Q N T = 0.55 W *s 3B5.5 + 1.05ft h = 122.05 - 47.2 iog T W* 2.594 X 1.05* h - 47.2 log H - 19.54 is mounted on a blank card for convenient handling, as illustrated in Fig. 3. 7. Procedure 7.1 Prepare a hiding standard as described in 6.4, or use the standard supplied with the logicator test charts. N' I --Strong colors were measured according to this test method using standards prepared with the self-same coatings. Some measure ments were also made using the regular white standard. Due to poor correlation in these tests it was decided to exclude strong colots from the scope of the test method. However, should measurements with such colors be attempted anyway, it is of interest to note that the white standard apparently served as well fdr that purpose as a standard made with the identical color. 7.2 Place a test chart on the vacuum plate. Then place the logicator at the top of the chart with its arms extending toward the operator. 7.3 Spread about 6 mL of the test paint evenly in front of the logicator, then draw down the full length of the chart (about 10 in. (254 mm)) at a uniform speed such that the total drawdown time is about 2.5 to 3 s. 7.4 Promptly after film application, determine the Wet Hiding Index (hsw) in accordance with 7.5. 7.5 Observation ofthe Hiding Index (hj: 7.5.1 Place the chart vertically in a well-illuminated glare-free location. 7.5.2 Hold the hiding standard next to the chart and identify by number the stripe that the standard matches in contrast. This number is the Hiding Index. 7.5.3 Ifthere is no exact match and it is difficult to decide which of two adjacent stripes is matched more closely, record their mean as the Hiding Index. However, if the standard is perceived as closer to one or the other of the two stripes, then report the Hiding Index as one more than the lower or one less than the higher, as the case may be. 7.6 Immediately after determining the Wet Hiding Index few), place the drawdown horizontally in a well-ventilated, dust-free location, as specified in Specification D 3924, and allow to dry for 40 to 48 h. Then repeat 7.5 to determine the Dry Hiding Index (ASD). 7.7 Make drawdowns in triplicate and calculate the mean index value to 0.1 units. Individual values that deviate from the mean by more than 1.5 units should be discarded and the test repeated. ; 3 Available from The Leneta Company, P.O. Box 86, H( >-Ho -Ku s , NJ 07423. s 4 A white standard of this description is supplied with the TGI 3 Logicator Test ^Inrts. 8. Calculation 8.1 Subtract the Wet Hiding Index, hsw from the Dry 889 DU PO 502 98069 # D 5007 TABLE 2 Logicator Scale Relationships Calculated from Equations in Table 1 index'4 Clearance Film Thickness0 Spreading Rate0 Index* Clearance Film Thickness0 h mils3 pm mils ffiVgat ma/L h mils nm mils urn 20 10*40 264 5.72 145 280 6.68 36 4.78 121 2,62 67 21 9.90 252 5.44 138 294 7.23 37 4.54 115 2.50 63 22 9.43 240 5.19 132 309 7.59 3B 4.32 110 2.38 60 23 8.98 228 4.94 126 325 7.97 39 4.12 105 2.26 58 24 6.56 217 4.71 120 341 6.37 40 3.92 100 2.16 .55 25 8.15 207 4.48 114 358 8.78 41 3.73 95 2.05 52 26 7.76 197 4.27 108 376 9.22 42 3.56 90 1.96 50 27 7.39 188 4.07 103 395 9.68 43 3.38 85 1.86 47 28 7.04 179 3.87 98 414 10.2 44 3.23 62 1.77 45 29 6.70 170 3.69 94 435 10.7 30 6.38 162 3.51 89 457 11.2 31 6.08 154 3.34 85 480 11.8 45 3.07 78 1.69 43 46 2.93 74 1.61 41 47 2.79 71 1.53 39 32 5.79 147 3.19 81 504 12.4 48 2.65 67 1.46 37 33 5.52 140 3.03 77 529 13.0 34 5.25 133 2.89 73 555 13.6 36 5.00 127 2.75 70 583 14.3 fl Boldface values refer to notches in TG19 Logicator. a Target values are significant to one decimal place. c Based on wet film thickness estimated at 55 SS of clearance. Spreading Rat, - tt2/gal 612 643 675 709 744 781 820 861 904 950 997 1047 1100 1S.iT 17,4 18.3 21 1 222 245 25.7 . 27,C Hiding Index, /?SD to obtain the wet-to-dry hiding change (WDHC), Ahs, as follows: WDHC = AAs = hSD - ftsW The value for WDHC is positive for an increase and negative for a decrease in hiding. To avoid possible misunderstanding write the sign of the change (+ or -) in every case. 8.2 If desired, calculate the corresponding percent change in wet-to-dry-hiding power as follows: WDHC% = (1.05WDHC - 1) x 100 9. Report 9.1 Report the following information: 9.1.1 The Wet-to-Dry Hiding Change (WDHC) in logicator units (LU) to one decimal place, as described in 8.1, and 9.2 If desired, the percent change in conventional hiding power (WDHC%), calculated as shown in 8.2.10 10. Precision and Bias 10.1 In an interlaboratory study of this test method, two operators in each of two laboratories and one operator in each of six laboratories, tested in triplicate five coatings with a wide range in wet-to-dry hiding change. Since the test -.< not repeated,the repeatability data is only for replicates. On, this basis the intralaboratory standard deviation was 0.77 11f with 85 df and the interlaboratory standard deviation was, I. 97 LU with 39 df. Based on these standard deviations ifcfollowing criteria should be used forjudging the acceptability of results at the 95 % confidence level: 10.1.1 Repeatability {Replicate)--Three replicates by the same operator should be considered suspect if they differ by more than 2.6 LU. 10.1.2 Reproducibility--Two results, each the mean ut-triplicates, obtained by different operators should be consid ered suspect if they differ by more than 5.7 LU. 10.2 Bias--This test method has no bias because there is no criterion for the property it measures more valid than the test method itself. N' 2--In the statistical analysis results were discarded on the following basis: (1) all results from one operator who appeared to be less sensitive than the other operators in detecting differences among triplicates, (2) one .replicate result from one laboratory because the. triplicate range was significantly higher than for other laboratories, and (3) all three results from the same laboratory for another paint, because the mean differed significantly from other means for that paint. II. Keywords 11.1 hiding power; wet-to-dry hiding change ll 890 DUPO 502 98070 DUP050298071 D5Q07 i; N' --For illustration only. Shading is not accurate. FIG. 3 Visual Hiding Standard The American Society for Testing and Materials takes no position respecting the validity ot any patent rights asserted In connection with any item mentioned In this standard. Users ot this standard are expressly advised that determination of the validity of any such patent rights, and (to risk of Infringement of such rights, ate entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and II not revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ot the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1918 Race St., Philadelphia, PA 19103. 892 DUP050298072 Designation: D 5009 - 89 Standard Test Method for Evaluating and Comparing Transfer Efficiency Under Laboratory Conditions1 This standard is issued under the fixed designation D 5009; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. ^ Scope BP.l This test method covers the evaluation and comparIn of the transfer efficiency of spray-applied coatings under ntrolled laboratory conditions. i.2 This test method has been shown to yield excellent [ffalaboratory reproducibility. Interlaboratory precision is orer and is highly dependent on closely controlled air flow ggge spray booth, the rate at which the paint is delivered to Impart, and other variables suggested in the test method. |f,3 Limitations: 1.3.1 This laboratory procedure only indicates the direojipn ofthe effect ofspray variables on transfer efficiency. The Bgnitude of the effect is determined only by specific plant S|erience. ' N' 1--This laboratory procedure requires specific equipment and B&eduics. For thosq laboratories that do not have apeess to the type of gjpupment required a more general laboratory procedure is being :|pared as Procedure B. 1.4 This standard may involve hazardous materials, oper- IJbipns, and equipment. This standard does not purport to \uddress all ofthe safety problems associated with its use. It is tfiie responsibility of the user of this 'standard to establish *appropriate safety and health practices and determine the ilicability of regulatory limitations prior to use. For "lc hazard statements, see Section 7 and Notes 2 and 3. 2. Referenced Documents !s2.1 ASTM Standards: D1200 Test Method for Viscosity by Ford Viscosity Cup12 D2369 Test Method for Volatile Content of Coatings2 D 3925 Practice for Sampling Liquid Paints and Related : Pigmented Coatings2 ' 2.2 National Fire Protection Association Documents3 NFPA 33 Spray Application Using Flammable arid Com- bustible'Materials i NFPA 86 Standard for Ovens and Furnaces , . Terminology 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 conveyor speed--the speed of the conveyor in centi? meters per minute during the test. 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint land Related Coatings and Materials and is the direct responsibility of Subcom|miuee D01.55 on Factory-Applied Coatings on Preformed, Products. Current edition approved October 27, 1989. Published December 1989. 2 Annual Book ofASTM Standards, Vol 06.01.' 3 Available from National Fire Protection Assn., Battery March Park, Quincy, yiMA 02269. 3.1.2 fluid massflow rate--the mass flow rate of paint in grams per minute during the test. 3.1.3 mass offoil--the weight of each target foil in grams before being painted. 3.1.4 mass offoil plus paint solids--the weight of each target foil in grams after being painted and baked. 3.1.5 mass ofpaint solids--the difference in the mass of the foils before painting and the mass of the foils after painting and baking. This is the sum of the mass Of the foil plus paint solids less the sum of the mass of the foil. 3.1.6 transfer efficiency--the ratio ofthe mass ofthe paint solids deposited on the foil to the mass of the paint solids sprayed during the test expressed as a percent. 3.1.7 weight percent solids--the solids content in percent of the total weight of a sample of the paint used during the test. 4. Summary of Test Method 4.1 Metal panels covered with preweighed aluminum foil are conveyed in a spraybodth past a fixed spraygun. The coated foils are then baked to remove volatile matter. The transfer efficiency is calculated on a weight basis using the solids content and quantity of the paint sprayed and the amount of solids on the coated aluminum foil target. 5. Significance and Use 5.1 Subject to.the limitations listed above, the procedure can be used as a research tool to optimize spray equipment and: paint formulations as well as to study the relative effect on transfer efficiency of changing operating variables, spray application equipment, and types of coatings. 6. Apparatus 6.1 Laboratory Scale, accurate to 0.001 g for weight percent, solids determination. 6.2 Platform Scale, accurate, or equivalent, to 0.01 g for mass of foil, mass of foil plus paint, and mass flow rate instrumentation calibration. 6.3 Mass Flow Rate Meter, or mass flow rate determina tion method, accurate to 2 % of the mass flow rate to be used during the test. 6.4 Conveyor Timer or conveyor timing method, accurate to 1 % of the conveyor speed to be used during the test. The equipment may consist of photoelectric cells or limit switches Used in conjunction with a digital timer or timing marks on the conveyor used in conjunction with a stop watch. Take at least two readings with a stopwatch and average the readings. 6.5 Targets, consisting of a set of ten steel panels 6 in. (15.2 cm) wide by 0.0625 in. (0.15875 cm) with 0.25-in. 893 DUP0502 98073 D 5009 (0.635-cm) radius corners. A minimum panel length of 48 in. (121.9 cm) should be used. The length ofthe panel should be set so that a minimum of 12 in. (30.4 cm) above and below the spray pattern is achieved. 6.5.1 It is essential to do this so that the entire height of the spray pattern is effectively captured. 6.6 Aluminum Foil, medium temper or equivalent, 1.5 mil (0.0037 cm) thick. 6.7 Back-Draw Water Wash Spray Booth, or equivalent. The booth should be a minimum of 6 ft (1.8 m) wide and capable of up to 120 ft/min (0.61 m/s) air velocity in the middle at the plane of the target. If a dry filter booth is used, filters should be'changed as necessary to. maintain uniform air velocity.: 6.8 Adjustable Rate Overhead Conveyor System, capable of hanging targets as specified, and capable of up to 40 ft/min (0.20 m/s) or the maximum speed desired by the user. 6.9 Forced Draft Curing Oven, ofsufficient size for curing targets, and capable of achieving and maintaining the cure temperatures specified by the paint supplier. All ovens should conform to NFPA' 86. 6.10 Curing Rack. 6.11 Stopwatch. 6.12 Air Velocity Measurement Equipment. 6.13 Humidity and Temperature Measurement Equip ment. ' 6.14 Compressed Air Supply. 7. Hazards 7.1 Fpr specific hazard information and guidance, consult the supplier's Material Safety Data Sheet (MSDS) for the materials used.. .... 8. Procedure 8.1 Set up the spray apparatus paint supply and the mass flow measurement equipment in accordance with the manu facturer's instructions. 8.1.1 In accordance with Chapter 9-11 of NFPA 33, all electrically conductive objects in the spray area, except those objects reqiiired;by the process to be at high: voltage', shall .be adequately grounded. 8.2 Agitate paint, in a closed container at least 30 min before any paint samples are taken. 8.3 Using an airtight container take a paint grab sample from, the paint pot in accordance with Practice D 3925. . 8.4 Determine and record the following from the paint sample: - , . o 8.4.1 Viscosity determined in accordance with Test Method D 1200. 8.4.2 Weight percent solids determined in accordance with Test Method D 2369. If the baking temperature in Test Method D 2369 is inadequate, use the manufacturers recom mended cureschedule.i a- 8.4.3 Resistivity for the samples being applied electrostat ically (An ASTM method is under development). 8.5 Set up the conveyor speed measuring equipment. 8.6 Cut the aluminum foil to dimensions of 15 in. (38 cm) by approximately 50 in. (127 cm) or 2 in. (5 cm) longer than the length of the target panel. 8.7 Consecutively number each precut foil strip before weighing using a permanent marking pen. DIRECTION OF WRAPPING STEEL PANEL ALUMINUM FOIL ._ Scale: Nat To Scale , . FIG. 1 Foil Attachment Technique '; 2:{-15teom) u 8.8 Weigh each test foil strip and record the uncoated- weight and the foil number.' 8i9 Attach: the preweighed, labeled test foil to Six targeb \ using the technique''`Shown in Fig! 1. Attach the unlabele|` foil on four scavenger targets as shown in Fig. 1. 8.10 Mount the'foil covered targets in consecutive order'1' as shown in Fig. 2, with the foil seam on each target facing away from the sprMy gun.'- 8.10.1 If electrostatic equipment is being used the resist ance shall be less than 1 by 106 SI between the target and the earth ground in accordance with Chapter 9-8 of NFPA 33. 8.11 Adjust the following equipment operating paramc- . ters to the values desired for testing: 8.11.1 Paint fluid pressure (kilopascals) at spray gun. r 8.11.2 Atomizing air pressure (kilopascals) at spray gun. <| 8.11.3 Rotating atomizer head speed (revolutions ( > > minute) with and without paint fluidhow. ^ 8.11.4 Operating voltage (kilovolts) if electrostatic equip ment is used. , , -, , . , 8.11.5 Ambient air temperature (degree Celsius). 8.11.6 Paint fluid temperature (degree Celsius). 8.11.7 Booth air velocity (feet per minute). 8.11.8 Relative humidity (percent). 8.11.9 Spray gun to target distance (centimeters). N ' 2: Precaution--If electrostatic equipment is being used, the gun-to-target distance shall be at least twice the sparking distance in accordance with Chapter 9-7 of NFPA 33. 8.11.10 Conveyor speed (centimeters per second). 8.11.11 Fluid mass flow rate (grams per minute). 8.11.12 Set the cure time and temperature in accordant < with the manufacturer's instructions. 894 DUP050298074 D 5009 IWIWI FIG. 2 (11+tn) ' . ~ . F = FIXED T1MINS MARK M = MOVING TfttlNG MARK ' Target Configuration for Transfer Efficiency Determination ,12 For electrostatic spray equipment, measure the operng voltage and adjust it according to the manufacturer's actions. 8.13 Turn otr'the spray booth and conveyor. At, least 15 s,, efore the first scavenger target passes in front of the gun, on the paint spray equipment. Maintain uniform paint during the test. .13.1 If mass flow measurement is used, begin the flow -asurement at the leading edge of the first scavenger target [ stop the mass flow measurement at the trailing edge of I last scavenger target, 8.13.2 If mass flow measurement equipment is not availle use the following technique. Just before turning on the ay booth and the conveyor, spray the gun into a eweighed covered plastic container for a minimum of 30 s. s<N' 3: Precaution--In addition to other precautions, turn off all h voltage to electrostatic spray guns to prevent personal injury. 8.13.3 Immediately weigh the container with paint, calcu'e the flow rate, and record the result. Just after turning off e spray booth and conveyor, repeat this procedure. Avjage the two results to obtain the average flow rate for the 'It. j N' 4--A gallon plastic bottle with the top cut off to conveniently 1 around the front of the gun is recommended to use with the above jscedure. A large plastic beaker covered with plastic wrap with a hole imcheci in the center of the plastic wrap works also. [Turn off all air sources to the spray gun before using the above pocedure to prevent paint splattering out of the container. 8.14 Record the following data: 8.14.1 Application Equipment: 8.14.1.1 Paint fluid pressure (kilopascals) at the spray gun, 8.14.1.2 Atomizing air pressure (kilopascals) at the spray un, 8.14.1.3 Rotating atomizer head speed (revolutions per inute) with and without paint fluid flow, and 8.14.1.4 Operating voltage (kilovolts) if electrostatic `uipment is used. 8A4.2Spray Booth and Conveyor: 8.14.2.1 Ambient temperature (degrees Celsius), 8.14.2.2 Paint fluid temperature (degrees Ceisius), 8.14.2.3 Bjoofh. alp velocity,(foot, per minute)) .'. 8.14).2;4 Relative humidity (percent), 8.14.2.5 Spray gun to target distance (centimeters), 8.14.2.6 Conveyor speed (centimeters per minute), and 8.14.2.7 Fluid mass flow rate (grams per minute). 8.15 After the paint flow and the conveyor are stopped, remove the painted targets from the conveyor and ensure that no paint is lost. Measure the wet film thickness to ensure that the proper amount of paint has been applied and record the wet film thickness. 8.16 Securely hang the coated targets on oven racks so all painted surfaces are exposed for uniform drying. Insert the racks into the oven and bake at the recommended manufac turer's cure schedule. 8.17 Remove the targets from the oven and let cool. 8.18 Remove the foil from each target, weigh and record the coated weight, the foil number, the percent vertical film coverage, and the dry film thickness at the center of the spray pattern. 8.19 The mass of the paint solids deposited is the differ ence in the total weight of the foils before painting and the total weight of the foils after painting and baking. 9. Calculation 9.1 Calculate the transfer efficiency using the following equation: X = (100 x C x P)/(F x S x W) where: T = transfer efficiency, % C = conveyor speed, cm/min, P = mass of paint solids deposited, g, F = fluid delivery rate, g/min, S' = weight percent solids expressed as a decimal, and W = effective target width, 30.48 cm. 895 DUP050298075 ________ D 5009 10. Report 10.1 Report the following information: 10.1.1 Transfer efficiency results, 10.1.2 Type of spray equipment, 10.1.3 Type of paint applied, 10.1.4 Paint application conditions, and 10.1.5 Conditions of test other than those specified in the procedure section of this test method. 11. Precision 11.1 This test method is derived from a study and report of transfer efficiency measurements conducted for the U. S. Environmental Protection Agency.4 The procedure de scribed was subjected to round-robin evaluation following ASTM guidelines. The procedure was used at eight laborato ries and results were obtained using conventional airless, 4 Development of Proposed Standard Test Methodfor Spray Painting Transfer Efficiency, Vols l and II, EPA Publication Nos. EPA-600/2-88-026a and EPA600/2-88-026b, Environmental Protection Agency, Research Triangle Park, NC. electrostatic air spray, and conventional air spray equipment Statistical treatment of the results for the test sites and spray equipment type (gun) yields the following transfer efficiency results: y Type of Gun Conventional airless: Within laboratory Between laboratory Gun Total Electrostatic Air Spray: Within laboratory Between laboratory Gun Total Conventional Air Spray: Within laboratory Between laboratory Gun Total 1.22 26.41 6.22 33.85 3.63 72.02 13.01 88.66 2.30 42.90 0.88 46.08 Standard Deviation 1.10 12. Keywords 12.1 laboratory method; spray applied coatings; transfei efficiency r/ia American Society for Testing and Materials takes no position respecting tha validity of anypatent rights asserted in connection with any Hem mentioned in this standard. Users ol this standard are expressly advised that determination at tha validity of any such patent rights, and the risk of Infringement ol such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and ifnot revised, either reapprovedor withdrawn. Your comments are invHed eitherforrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. r4 '! 896 DUP050298076 Designation: D 5010 - 91 Standard Guide for Testing Printing Inks and Related Materials*1 This standard is issued under the fixed designation D 50 JO: the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. I. Scope 1.1This guide covers a list of test methods, practices, and specifications that can be used-for the testing and evaluation af printing inks, printed ink films, and substrates used in iheir production (see Table 1). II. 2 This guide includes methods that were developed to lest paints, paint films, and substrates, but may be adapted or se in testing printing inks and printed matter. Tests on taw materials and analytical methods in general have not been included. It ||N' 1--For the purpose of this guide, clear coatings such as ^verprint varnishes are classed as printing inks. 1.3Other ASTM standards not specified here may also be Applicable. | Terminology ' 2.1 Definitions: 1-2.1.1 printing ink--a colored or pigmented liquid or paste [position that dries to a solid film after application as a layer by printing machinery. j2.1.1.1 Discussion--Printing inks may contain vehicles, lorants, waxes, solvents, and other additives. Bulk inks are :ed for dispersion, tinting strength, density, heat and ge stability, rheology, and printing properties. 2.1.2 printed inkfilm--thin layer of a printing ink deposonto a substrate by means of a laboratory or production [ting press, occasionally by a drawdown or roll-out iniqtre. Printed matter is the usual medium by which inks tested for appearance properties, drying, and resistance to ,ous agents. I;p This guide is under the jurisdiction of the ASTM Committee D-l on Paint I Related Coatings and Materials and is the direct responsibility of Subcom ee DO 1.56 on Printing Inks. Current edition approved May 15, 1991. Published July 1991. 2.1.3 printing substrate--material onto which ink is de posited in the production of printed matter. Printing sub strates include paper, paperboard, plastic film, glass, and metallic surfaces. In this guide, standards relating to sub strates are largely restricted to properties associated with appearance and printabiiity. 3. Test Categories 3.1 For convenience in selection, the test methods, prac tices, and specifications, listed in this guide are classified into three groups by type of printing process and in subgroups indicating whether the test is conducted on a bulk ink, a printed ink film, or a substrate (see Table 2). The group is given in the left column preceding the test method reference. The classification are a follows; 3.1.1 Group1--Applicable in GeneralClass A--Bulk inks. Class B--Printed ink films. Class C--Substrates. 3.1.2 Group 2--Applicable to Low Viscosity or Liquid Inks Associated With Flexography or Gravure: Class A--Bulk inks. Class B--Printed ink films. Class C--Substrates. 3.1.3 Group 3--Applicable to High Viscosity or Paste Inks Associated With Letterpress, Lithography, or Silk Screen: Class /(--Bulk inks. Class B--Printed ink films. Class C--Substrates. 4. Precision and Bias 4.1 If available, precision for each test method listed can be found in the latest revision of that test method, 5. Keywords 5.1 printed matter; printing inks; printing substrates; test methods and practices (tabulation of) 897 ASTM Designation D16 D56 D93 D185 D344 D 523 D 528 D562 D 644 D685 D724 D780 D 669 D918 D 971 D 1200 D1210 D 1259 D1310 D 1316 D1331 D1353 01474 D 1475 D 1535 D1544 D 1545 D 1590 D 1640 D 1644 D 1647 D1653 D 1725 D 1729 D 1849 D 1963 0 2066 D 2091 D 2196 D 2243 D. 2244 D 2248 D 2337 D 2369 O 2462 D 2574 D 2578 D 2616 D 2620 D 2794 0 2805 D 3134 D 3258 D3278 D 3359 D 3353 D 3424 D 3732 D 3825 D 3628 D 3924 D 3925 D 3928 D 3934 Volume 06.01 06.02 06.03 05.03 06.03 04.09 05.01 06.03 06.01 06.01 06.01 15.09 06.01 15.09 15.09 15.09 15.09 06.01 15.09 05.01 10.03 06.01 06.01 06.02 05.01 06.03 06.01 15.04 06:03 06.01 06.01 06.01 06.01 06.02 06.03 06.01 11.01 06.01 06.01 06.01 06.01 06.02 06.01 06.01 06.03 06.01 06.01 06-01 06.01 06.01 06.01 06.01 06.01 15.09 06.01 08.02 06.01 14.02 06.01 06.01 06.01 06.01 06.01 06.03 06.01 06.01 06.01 06.01 05.03 05.03 06.01 06.01 06.01 06.03 <} D 5010 TABLE 1 Numerical Listing of Ink-Reiated Standards Title Terminology Relating to Paint, Varnish, Lacquer, and Related Products Test Method for Flash Point by Tag Closed Tester Test Method for Flash Point by Pensky-Martin Closed Tester' Test Methods for Coarse Particles in Pigments, Pastes, and Paints Test Method for Relative Dry Hiding Power of Paints by the Visual Evaluation of Brushouts Test Method for Specular Gloss Test Method for Machine Direction of Paper and Paperboard Test Method for Consistency of Paints Using the Stormer Viscometer Test Method for Moisture Content of Paper and Paperboard by Oven Drying Method for Conditioning Paper and Paperboard Products for Testing Test Method tor Surface Wettability of Paper (Angle-of-Contact Method) Test Method tor Printing Ink Permeation of Paper {Castor Oil Test) Test Method for Evaluating the Degree of Settling of Paint Test Method for Blocking Resistance of Paper surd Paperboard Test Method for Interfacial Tension of Oil Against Water by the Ring Method Test Method for Viscosity by Ford Viscosity Cup Test Method for Fineness of Dispersion of Pigment-Vehicle Systems Test Methods for Nonvolatile Content of Resin Solutions Test Method for Flash Point and Fire Point of Liquids by Tag Open-Cup Apparatus m Test. Method for Fineness of Grind of Printing Inks by the NPIRl Grindometer Test Methods for Surface and Interfacial Tension of Solutions of Surface-Active Agents Test Method for Nonvolatile Matter in Volatile Solvents for Use In Paint, Varnfsh, Lacquer, and Related Prodjets's Test Methods for Indentation Hardness of Organic Coatings Test Method for Density of Paint, Varnish, Lacquer, and Related Products Test Method for Specifying Color by the Munsell System Test Method for Color of Transparent Liquids (Gardner Color Scale) Test Method for Viscosity of Transparent Liquids by 8ubble Tlme Method Test Methods for Surface Tension of Water and Waste Water Test Methods for Drying, Curing, or Film Formation of Organic Coatings at Room Temperature Test Methods for Nonvolatile Content of Varnishes Test Methods for Resistance of Dried Films of Varnishes to Water and Alkali Test Methods for Water Vapor Permeability of Organic Coating Films Test Method for Viscosity of Resin Solutions , , Practice tor Visual Evaluation of Color Differences of Opaque Materials Test Method for Package Stability of Paint Test Method for Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25C Test Methods for Relative Tinting Strength of Printing-Ink Dispersions Test Method for Print Resistance of Lacquers Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield) Viscometer Test Method for Freeze-Thaw Resistance of Water-Borne Coatings Test Method for Calculation of Color Differences from Instrumental^ Measured Color Coordinates Practice for Detergent Resistance of Organic Finishes Test'Method for Freeze-Thaw Stability of Multicolor Lacquers Test Method for Volatile Content of Coatings Method for Wax Pick Test for Surfaoe Strength of Paper Test Method for Resistance of Emulsion Paints in the Container to Attack by Microorganisms Test Method for Wetting Tension of Polyethylene and Polypropylene Films Test Method for Evaluation of Visual Color Difference with a Gray Scale / Test Method for Light Stability of Clear Coatings Test Method for Resistance of Organic Coatings to the Effects of Rapid Oeforrnation (impact) Test Method for Hiding Power of Paints by Reflectometry Practice for Establishing Color and Gloss Tolerances Test Method for Porosity of Paint Rims Test Methods for Flash Point of Liquids by Setaflash Closed-Cup Apparatus Test Methods for Measuring Adhesion by Tape Test Test Method for Film Hardness by Pencil Test Method of Evaluating the Ughtfastness of Printed Matter Practice for Reporting Cure Times of Ultraviolet-Cured Coatings Test Method for Dynamic Surface Tension by the Fast Bubble Technique Test Method for Flash Point by Setaflash Closed Tester Specification for Standard Environment for Conditioning and Testing Paint, Varnish, Lacquers, and Related Materials Practice for Sampling Liquid Paints and Related Pigmented Coatings Test Method for Evaluation of Gloss or Sheen Uniformity Test Method for Flash/No Flash Test--Equilibrium Method by a Closed-Cup Apparatus 898 DUP050298078 ASTM Designation lrgT D 3960 D 4017 D 4040 D 4060 D 4086 D 4141 HF D 4144 K D 4212 $ D4287 % ll 1 Jjlj*,* D 4302 D4359 D4361 D 4366 D 4449 D 4459 m llr^* ilv D 4518 D 4541 D 4674 SI1' w. D 4713 D 4758 D 4942 D.5039 D 5067 D5C98 97 o & jjjjf Pr fllg|V nfi afe* Pi Sr Blip. So t ', flmf-~ Bra mmi B i 284 E 308 313 E 429 430 E 691 <' E 805 E 991 E 1331 E 1347 E 1349 F3A F 149 F 151 F 372 F 413 F 425 F 909 F 1125 G7 G 23 nw b ro' G 24 G 26 Volume 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06,01 06.01 08.03 06.01 06.01 08.03 06.01 06.02 06.01 15.09 06.01 06.01 '06.01 14.02 15.09 14.02 14.02 14.02 14.02 06.01 06.03 08.03 14.02 14.02 14.02 14.02 14.02 14.02 15.09 15.09 15.09 15.09 15.09 15.09 15.09 15.09 14.02 06.01 07.02 08.03 14.02 07.02 14.02 06.01 08.03 14.02 # D 5010 TABLE 1 Continued Title Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings Test Method for Water In Paints and Paint Materials by Karl Fischer Method Test Method for Viscosity of Printing Inks and Vehicles by the Falling-Rod Viscometer Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser Practice for Visual Evaluation of Metamerism Practice for Conducting Accelerated Outdoor Exposure Tests of Coatings Method tor Estimating Package Stability of Coatings for Ultraviolet Curing Test Method for Viscosity by Dip-Type Viscosity Cups Test Method for High-Shear Viscosity Using tha ICI Cone/Plate Viscometer Specification for Artists' Oil, Resin-Oil, and Alkyd Paints Test Method for Determining Whether a Material is a Liquid or a Solid Test Method for Apparent Tack of Printing Inks and Vehicles by the lnkometer Test Methods for Hardness of Organic Coatings by Pendulum Damping Tests Test Method for Visual Evaluation of Gloss Differences Between Surfaces of Similar Appearance Practice for Operating art 'Accelerated Lightfffitness Xenon-Arc-Type (Water Cooled) Light-Exposure Apparatus for the Exposure of Plastics for Indoor Applications Test Methods for Measuring State Friction of Coating Surfaces Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers Test Method for Accelerated Testing for Color Stability of Plastics Exposed to Indoor Fluorescent Light and Window-Filtered Daylight < Test Methods for Nonvolatile Content of Printing inks, Resin Solutions, and Vehicles Test Method for Nonvolatile Content of Latexes Test Methods for Water Pickup of Lithographic Printing Inks and Vehicles In a Laboratory Mixer Methods for Identification of Wire Side of Paper Specification for Artists' Watercolor Paints Specification for Artists' Acrylic Emulsion Paints Test Method for Directional Reflectance Factor, .45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reffectometry : Definitions of Terms Relating to Appearance of Materials Method for Computing the Colors of Objects by Using the CIE System Test Method for Indexes of Whiteness and Yellowness of Near-White, Opaque Materials Method for Measurement and Calculation of Reflecting Characteristics of Metallic Surfaces Using Integrating Sphere Instruments Method for Measurement of Gloss of High-Gloss Surfaces by Goniophotometry Practice for Conducting an Interlaboratory Study to Determine the Precision of a-Test Method Practice for Identification of Instrumental Methods of.Color and Color-Difference Measurement of Materials Practice for Color Measurement of Fluorescent Specimens Test Method for Reflectance Factor and Color by Spectrophotometry Using Hemispherical Geometry Test Method for Color and Color Difference Measurement of Object-Color Specimens by Tristimulus (Filter) Colorimetry Test Method for Reflectance Factor and Color by Spectrophotometry Using Bidirectional Geometry Test Method for Liquid Extraction of Flexible Barrier Materials Definitions of Terms Relating to Optical Character Recognition Test Method for Residual Solvents in Flexible Barrier Materials Test Method for Water Vapor Transmission of Flexible Barrier Materials Using an Infrared Detector Technique Practice for Preparation of an Offset Duplicator for Use in Functional Testing of lithographic Copy Products Definitions of Terms Relating to Lithographic Copy Products Definitions of Terms Relating:to Printers Terminology of Image Quality in Impact Printing Systems Practice for Atmospheric Environmental Exposure Testing of NonmetaiHc Materials Practice for Operating Light-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Exposure of Nonmetaliic Materials Practice for Conducting Exposures to Daylight Filtered Through Glass Practice for Operating Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water lor Exposure of Nonmetaliic Materials 899 DUP050298079 Group 1 ABC 1C 1ABC 1A 1A0C 1A 1ABC 1ABC 1ABC 1ABC 1A 1ABC 1ABC 1ABC 1A8C 1ABC 1ABC 1C 1ABC 1ABC 1ABC 1ABC 1C 1ABC 1ABC 1ABC 1ABC IB IB 3A IB IB IB IB 1A 1A 1A 1A 1A IB IB # D 5010 TABLE 2 Index of Standards by Property Topic Testing in General Terminology Relating to Paint, Varnish, Lacquer, and Related Products - ASTM Designation D 16 Conditioning Paper and Paperboard Products for Testing Conditioning and Testing Paint, Varnish, Lacquer, and Related Materials, Standard Environment for Determining Whether a Material is a Liquid or a Solid Iniertaboratory Study to Determine the Precision of a Test Method D 685 D 3924 D4359 E 691 Sampling Liquid Paints and Related Pigmented Coatings Appearance Properties Terminology Relating to Appearance of Materials Color and Reflectance Calculation of Color Differences From Instrumental^ Measured Coordinates Color and Color-Difference-by Tristimuius (Filter) Colorimetry Color of Fluorescent Specimens Color of Transparent Uquids (Gardner Color Scale) D3925 E 284 D 2244 E 1347 E 991 D 1544 Computing the Color of Objects by the CIE System Directional Reflectance Factor, 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry Establishing Color and Gloss Tolerances Identification of Instrumental Methods of Color or Cbior-Difference Measurement of Materials Reflectance Factor and Color by Spectrophotometry Using Bidirectional Geometry Reflectance Factor and Color by Spectrophotometry Using Hemispherical Geometry Reflecting Characteristics of Metallic Surfaces Using Integrating-Sphere Instruments Specifying Color by the Munsell System Visual Color Difference With a Gray Scafe Visual Evaluation of Color Differences of Opaque Materials Visual Evaluation of Metamerism Whiteness and Yellowness of NearWYhtte Opaque Materials . . Gloss Gloss of High-Gloss Surfaces by Goniophotometry Specular Gfoss (20, 60, 85) Visual Evaluation of Gloss Differences. Between Surfaces of Similar Appearance Visual Evaluation of Gloss or Sheen Uniformity Opacity and Strength Hiding Power of Paints by Reflectometry Relative Hiding Power of Paints by the Visual Evaluation of Brushoute Relative Tinting Strength of Printing Ink Dispersions - Other Optical Properties Definitions of Terms Relating to Optical Character Recognition Terminology of Image Quality in Impact Printing Systems Chemical Resistance Detergent Resistance of Organic Finishes Resistance of Dried Films of Varnishes to Water and Alkali Density Density of Paint, Varnish. Lacquer, and Related Products Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials at 25/25*C Dispersion Coarse Particles in Pigments, Pastes, and Paints Fineness of Dispersion of Pigment-Vehicle Systems Fineness of Grind of Printing Inks by the NPIRI Grindometer Drying Dryffig, Curing, or Film Formation of Organic Coatings at Room Temperature Reporting Cure Times of Ultraviolet-Cured Coatings E308 E 97 D 3134 E 805 E1349 E 1331 E 429 :> D1535 D 2616 D 1729 D 4086 E 313 E 430 D 523 4449 D 3928 D2805 D344 D 2066 F 149 F 1125 D 2248 D 1647 01475 D1963 D 185 D1210 D1316 D 1640 D 3732 ASTM Volume"NoT~ 06.01 06.02 06.03 15.09 06.01 06.01 06.03 08.03 14.02 06.01 14.02 06-01 14.02 14.02 06.01 06.02 06.03 14.02 06.01 14.02 15.09 06.01 14.02 14.02 14.02 14.02 06.01 06.01 06.01 06.01 14.02 06.01 14.02 06.01 06.01 06.01 08.01 06.01 06.01 15.09 15.09 06.01 06.01 06.01 06.03 06.01 06.01 06.01 06.01 06.01 900 . __.______ -- DUP050298080 T : Group S' R 1A tj- 1A * 1A i 1A li 1A A 1C ? 1A 1 2A 1A ' 1A 1A l 1A r 1A 1A . J IB IB r 1B IB IS \ IB 9 l IB * IB IB 1 IB 1 IB IB IB IB IB IB IB IB IB IB 15 IB IB 2C 3A IB 1C 1C 3AC 1C 3A 3C 1C D 5010 TABLE 2 Continued Topic Heat Stability Flash/No Flash Test--Equilibrium Method by a Closed-Cup Apparatus Flash Point by Pensky-Marlin Closed Tester ASTM Designation D 3934 D 93 Flash Point of Liquids by Setafiash Closed-Cup Apparatus Flash Point by Setafiash Closed Tester Flash Point by Tag Closed Tester Moisture Content of Paper and Paperboard by Oven Drying Rash Point and Fire Point by Tag Open-Cup Apparatus Nonvolatile Content of Latexes Nonvolatile Content in Printing Inks, Resin Solutions, and Vehicles Nonvolatile Content of Resin Solutions Nonvolatile Content of Varnishes Nonvolatile Matter in Volatile Solvents for Lise in Paint. Varnish, Lacquer, and Related Products Volatile Content of Coatings Volatile Organic Compound (VOC) Content of Paints and Related Coatings Light and Weather Fastness Accelerated Outdoor Exposure Test of Coatings Accelerated Testing for Color Stability of Plastics Exposed to indoor Fluorescent Lighting and Window-Filtered Daylight Atmospheric Environmental Exposure Testing of Norimetallic Materials Light Stability of Clear Coatings Ughtfastness of Printed Matter Natural Light Exposures Under Glass Operating an Accelerated Ughtfastness Xenon-Arc-Type {Water Cooled) Light-Exposure Apparatus for the Exposure of Plastics for Indoor Applications Operating Ught-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Exposure of Nonmetallfc Materials D 3276 D3828 D56 D 644 D 1310 D4758 D4713 01259 D1544 D1353 D 2369 D 3960 D 4141 D 4674 ' G7 D2620 D3424 G24 D 4459 G'23 Operating Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water for.Exposure of Nonmetallic Materials Specification for (Ughtfastness of) Artists' Oil, Resin-Oil, and Alkyd Paints Specification for (Ughtfastness of) Artists' Wateroolor Paints Specification for (Ughtfastness of) Artists*' Acrylc Emulsion Paints Physical Strength and Resistance (Nonchemical) Abrasion Resistance of Organic Coatings by Taber Abraser Adhesion by Tape Test Film Hardness (of Organic Coatings) by Pencil Test Hardness of Organic Coatings by Pendulum Damping Test indentation Hardness of Organic Coatings Print (Imprint) Resistance of Lacquers Pull-off Strength of Coatings Using Portable Adhesion Tester Resistance of Organic Coatings to the Effects of Rapid Deformation (Impact) Static Friction of Crating Surfaces Porosity and Permeability Porosity of Paint Films Water Vapor Permeability of Organic Coating Films Water Vapor Transmission Rate of Flexible Barrier Materials Using an Infrared Detection Technique Printing Properties Definitions of Terms Relating to Lithographic Copy Products Definitions of Terms Relating to Printers Blocking Resistance of Paper and Paperboard Machine Direction of Paper and Paperboard Preparation of an Offset Duplicator for Use fn Functional Testing of Lithographic Copy Products Printing Ink Permeation of Paper (Castor Oil Test) Water Pickup of Lithographic Printing Inks and Vehicles in a Laboratory Mixer Wax Pick Test for Surface Strength of Paper Wire Side of Paper G 26 D 4302 D 5067 5096 D 4060 0 3369 D 3363 D 4366 D 1474 D 2091 D4541 D 2794 D4518 D 3258 D 1653 F 372 F 425 F 909 D918 D 528 F 413 D 780 D 4942 D 2482 D5039 ASTM Volume No. 06.03 04.09 05.01 06.03 06.03 05.03 05.01 06.03 15.09 05.01 06.03 06.02 06.01 06.02 06.01 06.03 06.01 06.01 06.01 08.03 14.02 06.01 06.01 07.02 14.02 08.03 06.01 07.02 08.03 14.02 06.01 08.03 14.02 06.01 D6.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06.01 06,01 06.01 06.01 06.01 15.09 15.09 15.09 15.09 15.09 15.09 15.09 06.01 15.09 15.09 901 mm DUP0502 98081 D 5010 Group 3A 1A TA 1A 2A 1A 3A 1A iA V 2A 1A 1A. 1A 2A 1A 1A 1A 1A 1C 2C 2C 2C 1A TABLE 2 Continued Tope Rheology Apparent Tack of Printing Inks and Vehicles by the Inkometer Consistency of Paints Using the Stormer Viscometer High-Shear Viscosity Using the ICI Cone/Plate Viscometer Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield) Viscometer Viscosity by Dtp-Type Viscosity Cups Viscosity by Ford Viscosity Cup Viscosity of Printing Inks and Vehicles by the Falling-Rod Viscometer Viscosity of Resin Solutions Viscosity of Transparent Liquids by Bubble Time Method Storage Stability Degree of.Settiing of Paint Freeze-Tnaw Resistance Cf Water-Borne Paints Freeze-Thaw Stability of Multicolor Lacquers Package Stability of Coatings for Ultraviolet Curing Package Stability of Paint Resistance of Emulsion Paints in the Container to Attack by Microorganisms Surface Chemistry Dynamic Surface Tension by the Fast Bubble Technique Interfacial Tension of Oil Against Water by the Ring Method Surface and Interfacial Tension of Solutions of Surface-Active Agents Surface Tension of Water and Waste Water Surface Wettability of Paper {Angle-of-Contact Method) Wetting Tension of Polyethylene and Polypropylene Films Special Analytical Tests Liquid Extraction of Flexible Barrier Materials Residual Solvents in Flexible Barrier Materials Water in Paints and Paint Materials by Karl Fischer Method ASTM Designation ASTM Volume~No~ D4361 D 562 D 4267 D 2196 D 4212 D 1200 D 40f40 D 1725 D 1545 06.01 06.01 06.01 06.01 05.01 06.01 06.01 06.02 06.01 D 869 D 2243 D 2337 D 4144 D 1849 D 2574 06.01 06.01 06.01 06.01 06.01 06.01 D 3825 D 971 D1331 ' D 1590 D 724 D 2578 05.03 05.01 15.04 11.01 15.09 08.02 F 34 F151 D 4017 15.09 15.09 06.01 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights> and the risk of infringement of sue* rights, are entirely their own responsibility. This standard ^ subject to revision at any time by the responsible technical comrpitteeand must be reviewed every five years and if not revised, either reapproved or withdrawn, Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters, Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feef that your comments have hot received e fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. BJj||op^' *if`T VP-'- av HP** |jp>l| Slag ip .i Mgyl apiii i'll . faints J ,\oia IPH llipi grfrijn j ftUMldl j 902 DUP050298082 . # Designation: D 5031 - 89 Standard Practice for Conducting Tests on Paints and Related Coatings and Materials Using Enclosed Carbon-Arc Light and Water Exposure Apparatus1 This standard is issued under the fixed designation D 5031; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon U) indicates an editorial change since the last revision or reapproval. '! ^1? Scope r? 1.1 This practice covers accelerated exposure testing of {.-'paint, varnish, lacquer, and related products. The apparatus iCJw fcs available are single enclosed carbon arcs (Types H and J?HH) and twin enclosed carbon arcs (types D and DH). Both .'types are manufactured with or without automatic humidity ^control.2 Table 1 describes commonly used test conditions, rlaboratory comparisons must only be' made using the s device type and test conditions. Jp The procedures described ip this practice were pievi|y included in Practice ,D 822, which covered the use of filtered open flame and enclosed asarbon arcs fortesting ;ts, varnishes, lacquers, and related products. SJ' 1--Another procedure for exposing these products is covered SPractice D 3361, in which the specimens are subjected to radiation ! i an unfiltered open-flame carbon arc that produces much higher ils ofshort wavelength radiation than filtered open-flame or enclosed bon arcs. Only automatic humidity controlled open-flame carbon-arc jjjratus (Type EH) is applicable to Practice D 3361. lj-3, This standard does not purport to address all of the mty problems associated with its use. it is the responsibility ithe user ofthis standard to establish appropriate safety and jjpft/t practices and determine the applicability ofregulatory nitations prior to use. For specific hazard statements, see etion 4. 'Referenced Documents ASTM Standards: >358 Specification for Wood to Be Used as Panels in Weathering Tests of Coatings3 jj&523 Test Method for Specular Gloss3 > 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products3 1610 Test Methods for Evaluating Degree of Rusting on Painted Steel Surfaces3 I 659 Method of Evaluating Degree of Chalking of Exterior Paints3 | 660 Test Method for Evaluating Degree of Checking of Exterior Paints3 IfThis practice is under the jurisdiction of ASTM Committee D-l on Paint and jjpated Coatings and Materials and is the direct responsibility of Subcommittee j$i27 on Accelerated Testing. ^Current edition approved Dec. 29, 1989. Published April 1990. p;Apparatus and carbon arcs manufactured by Atlas Electric Devices Company, ||4 N. Ravenswood Avenue, Chicago, [L 60$ 13 have been found satisfactory for Ipurposc. M Annual Book ofASTM Standards, Voi 06.01. D661 Test Method for Evaluating Degree of Cracking of Exterior Paints3 D662 Test Method for Evaluating Degree of.Erosion of Exterior Paints3 D714 Test Method for Evaluating Degree of Blistering of Paints3 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints3 D822 Practice for Conducting Tests on Paint and Related Coatings and Materials using Filtered Qpen-Flame. Car bon-Arc Light and Water Exposure Apparatus3 D823 Test Methods for Producing Filins of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 D1005 Test Methods for Measurement of Dry-Film Thickness of Organic Coatings Using Micrometers3 D1186 Test Methods for Nondestructive Measurement of,' Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base3 - -. D1400 Test Method for Nondestructive Measurement <of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base3 D 1729 Practice for Visual Evaluation ofColor Differences of Opaque Materials4 D 1730 Practices for Preparation of Aluminum and Alu minum-Alloy Surfaces for Painting5 . D 2244 Test Method for Calculation of Color Differences from Instmmentally Measured Color Coordinates3 D2616 Test Method for Evaluation of Visual Color Difference with a Gray. Scale4 D 3361 Practice for Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Flame- Carbon-Arc Type) for Testing Paint,' Varnish, Lacquer, and Related Prod ucts Using, the Dew Cycle3 D 4214 Test Methods for Evaluating Degree ofChalking of Exterior Paint Films3 E 97 Test .Method for Directional Reflectance Factor, ,45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Refleetometry6 G23 Practice, for Operating Light- and Water-Exposure Apparatus (Carbon-Arc Type) With and Without Water - for Exposure of Npnmetallic Materials6 * Annual Book ofASTM Standards, Vol i4.02. 5 Annual Book ofASTM Standards, Vols 02.05 and 06.01. 6 Annual Book of ASTM Standards, Vols 06.01 and 14.02. 903 DUP050298083 # D 5031 TABLE 1 Cycles Commonly Used for Testing Paints, Varnishes, Lacquers, and Related Coatings In Enclosed Carbon-Arc Devices Cycle Description 102 miri light 1$ miH light and water spray 18 li using: 102 mill light IB rtllri light and water spray 6 h at 95 4 % relative humidity with no water spray 48 rhin light 12 min'.light and water spray 4h light 4 H water spray f2 h light 12 h water spray 8 h light 10 h iight and water spray Black Panel Temp/ F <C) Typical Uses 145 5 (63 2.5) general coatings 145 5 (63 2.5) 75 3 general coatings 145 5 (63 2.5) 145 5 (63 2.5) 145 5 (63 2.5) 145 5 (63 2.5) original equipment manufactored coalings exterior pigmented paints exterior wood stains and clears marine enamels 6 h Water spray , A Unless otherwise indicated, black panel temperature during light only portion of tie cycle. B.Historical convention has established this as a very commonly used test cyde. 3. Significance and Use 3.1 This practice is intended to evaluate coating films for tlieir stability to ultraviolet light and moisture. If the spectral power distribution of the light source used for exposure tests does not adequately simulate that for terrestrial solar radia tion, it may produce a different type of degradation and distort the ranking of materials obtained in outdoor expo sures, Figures I and 2 compare representative spectral power distributions of a twin enclosed carbon arc with that of terrestrial sunlight. 3.2 No single operating procedure for light-exposure ap paratus with or without water can be specified as a direct simulation of natural exposure. This practice does not express, or imply, a specific correlation with outdoor expo sure. 3.3 Since natural environments vary with respect to climate, geography, and topography, it may be expected that the effects of natural exposures will vary accordingly. Fur thermore, all materials are not affected equally by the same environment. Therefore, results obtained by use of this practice should not be represented as equivalent to those of any natural weathering test until the degree of correlation has been empirically established for the material in question. 3.4 Variations in results are possible between instruments bf the same type operating within the accepted limits of this practice. It is recommended that results obtained using this practice be compared with those for a control or reference material that is mutually agreed upon by the interested parties. 3.5 All references to exposures in accordance with this practice must include a complete description ofthe test cycle used in addition to the type ofdevice used. 250 800 350 400 WAVELENGTH (nm) N' --The enclosed carbon-arc irradiance was measured at the sample plane I! at a position centered between the two carbon arcs. Sunlight was measured in ' Phoenix, AZ, at the summer solstice with clear sky at sotor noon using a double grating monochromator (1-nm bandpass) with a quartz cosine receptor on an equatorial fbllow-the-sun mount. Because of momentary fluctuations In intensity due to flickering of the carbon-arc flame, the spectral power distribution shown In this figure is relative and is not to be used to calculate or estimate total radiant exposure for tests In enclosed carbon-arc devices. FIG. 1 Representative Spectral Power Distributions (250-4QG flm) for Twin Enclosed Carbon Arcs and Terrestrial Sunlight Rhurf Twin Fnetosed Carbon Arc ; N' --Measurements were made as described in Fig. 1. Because of momen tary fluctuations in intensity due to flickering of the carbon-arc flame, the spectral power distribution shown in this figure is representative and is not meant tp be used to calculate or estimate total radiant exposure for tests In enclosed carbon-arc devices. FIG. 2 Representative Spectral Power Distributions (300-350 nm) for Twin Enclosed Carbon Arcs and Terrestrial Sunlight 4. Hazards 4.1 Precaution--In addition to other precautions, never look directly at the carbon arc because ultraviolet radiatiun can damage the eye. Most carbon-arc machines are equipped with door safety switches, but users of old equipment must be certain to turn the OPERATE switch OFF before opening the test-chamber door. 4.2 The burning carbon rods used in these devices become very hot during use. Make sure to allow at least 15 min for the arcs to cool after the device is turned off before 904 DUP050298084 # D 5031 empting to change the carbon rods. Avoid inhaling ash st when changing carbon rods. Test Specimens 5.1 Apply the coating to flat (plane) panels with the Ulubstrate, method of preparation, method of application, Lcoating system, film thickness, and method of drying consis tent with the anticipated end use, or as mutually agreed upon gbetween the producer and user. I, 5.2 Panel specifications and methods of preparation in clude but are not limited to Methods D 609, Specification =J;358, or Practices D 1730. Select panel sizes suitable for use fj|fith the exposure apparatus. 5.3 Coat test panels in accordance with Test Methods 823 and measure the film thickness in accordance with an ippropriate procedure selected from Test Methods D 1005, '1186, or D 1400. Nondestructive methods are preferred llpcause panels so measured need not be repaired. Prior to exposing coated panels in the apparatus, Condition them at 73 3"F (23 2C) and 50 5 % relative ! uunidity for one of the following periods in accordance with ffiic type of coating: & j8|:; Baked coatings Radiation-cured coatings All other coatings 24 h 24 h 7days N' 2--The procedures and specifications described in 5.2 through jjjf-'.M are recommended but others may be used if agreed upon by all `^interested parties. 3 jjU6. Procedure af-.*}, 6.1 Mount the test specimens both above and below a ^horizontal plane at the center of the single arc or centered pjbetween the two enclosed carbon arcs. When the exposure fc.interval does not exceed 24 h, locate each specimen equidis Eant from the horizontal plane at the center of the single arc of centered between the arcs. if ' 6.2 To ensure uniform exposure conditions for all specigjtiiens, reposition them vertically within their holders in a j||gquence that will provide each specimen with equivalent pposure periods in each location. For exposure intervals not Exceeding 100 h, reposition specimens daily. For longer Wpposures, reposition specimens weekly. Other methods of ff-acnieving uniform total irradiation may be employed if 3 ggnutually agreed upon between all concerned parties, i Ip, 6.3 Table 1 lists test-cycle conditions commonly used for evaluation of paints, varnishes, lacquers, and related coat- - JV' T}7` 6.4 It is recommended that the temperature of the water SLiised for specimen spray be 60 9F (16 5"C). Water used for specimen spray must meet the purity levels specified in Practice G 23 in order to avoid unrealistic water spotting. 6.5 When mutually agreed upon, cycles other than those listed in Table 1 may be used. The term cycle is defined as the set of exposure conditions (light, light plus water spray, dark periods) that are repeated. 7. Periods of Exposure 7.1 Use one of the following methods to determine the duration of the exposure under this practice: 7.1.1 A mutually agreed upon specified number of total hours. 7.1.2 The number of total hours of exposure required to produce a mutually agreed upon amount of change in either the test specimen or an agreed upon control or reference material. 8. Evaluation of Specimens After Exposure 8.1 Evaluate or rate changes in exposed test specimens in accordance with Test Methods D 523, D 610, D 659, D 660. D 661, D 662, D 714, D 772, D 2244, D 2616, D 4214, E 97, and Practice D 1729. Consider product use requirements when selecting appropriate methods. 8.2 Evaluate test specimens by ranking their performance relative to a control or reference material exposed at the same time. 8.3 Plot properties of test specimens and controls as a function of exposure time and compare rate of change with that of the control or reference material. When this method of evaluation is used, the control or reference material must be exposed at the same time and in the same device as the test specimens. 8.4 Other methods for evaluating test specimens may be used if mutually agreed on by all interested parties. 9. Report 9.1 Report the following information: 9.1.1 Complete description of exposure procedure-used, including: 9.1.1.1 Light/light plus water/dark cycle used, type of device used (single or twin enclosed carbon arc), 9.1.1.2 Operating black panel temperature during ail portions of exposure cycle, 9.1.1.3 Operating relative humidity, and 9.1.1.4 Temperature of water used for water spray. 9.1.2 Total hours of test. 9.1.3 Test specimen preparation. 9.1.4 Identification of controls used. 9.1.5 Results of evaluation test or tests performed on specimens and control or standard samples. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of infringement of such rights', are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if rtot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, ft you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 905 DUP050298085 Designation: D 5043 - 90 Standard Test Methods for Field Identification of Coatings1 This siandard is issued under the fjxcd designation D 5043; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the yearoflnst revision. A number in parentheses indicates the year of last rcapproval. A superscript epsilon (i) indicates an editorial change since the last revision or rcapproval. 1. Scope 1.1 These test methods cover procedures and portable apparatus for determining the generic type of coating Films most likely to be encountered on structures. The coating can either be weathered from exposure or be freshly applied. 1.2 Most commonly used coatings can be divided into the broad categories and subgroups shown in Table 1 on the basis of the nonvolatile component (generic types) of their vehicle .(film forming resin, binder). Although the curing, of some coatings involves more than one process and coatings may contain more than, one type of resin, they can usually be assigned to one of the basic classes and generic types listed in Table l, 1.3 For field exposed coatings, it is suggested that these test methods be used as part of a complete evaluation of a coated surface as it is frequently helpful to consider the environment of exposure and how the coating has performed in the environment when drawing conclusions from these tests.. 1.4 These test methods will not result in the identification of components of a coating beyond general classification of the coating by generic type and are not appropriate if more detailed analysis is required, far example, as a part of failure analysis of to identify between different manufacturers of the same type of coating. They also may not be definitive enough to identify complex systems that include .multiple layers ofdifferent generic types of coatings. 1.5 The evaluation of results is quite subjective. Practice and experience are required to minimize misinterpretation. Repeat tests may be required.. 1.6 None of the tests is to be taken alone as grounds for identifying the generic type. Only the combination of results from several or all of the tests are to be used in conclusions regarding generic types. . 1.7 This standard does not purport to address all of the safely problems associated with its use. It is the responsibility ofthe user ofthis standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use: For specific hazard statements, see Notes 8, 9, and 11. 2. Summary of Test Methods 2.1 Samples of coatings films are tested with solvents and chemicals and subjected to pyrolysis to provide evidence of their generic type. Figure 1 shows a flow chart for suggested order of tests and classification of results. 1 These test methods arc under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and are the direct responsibility of Subcommittee D0J.46 on Industrial Protective Coatings. Current edition approved April 27, 1990. Published June J990. 3. Significance and Use 3.1 Information about the generic type of coating on a surface is required to select compatible coatings for re painting and can be used when evaluating the performance of a coating in an environment in decisions on upgrading or replacing a coating system. These test methods provide information on generic type, can be performed in the field by personnel with limited laboratory experience, and require a minimum of equipment and materials. 4. Sampling 4.1 The sample of coating can be obtained by chipping < ( . scraping with a knife or by sanding and then brushing the material into a specimen container or clean envelope. Care should be taken not to cut into substrates, such as plastic or asphalt, that contain polymeric or bituminous materials Small portions of untreated wood, masonry, or steel do not ordinarily interfere with the tests. Some tests can be con- ' ducted directly on the coating surface. If a liquid sample of coating is to be evaluated, a film of the coating should first be * cast on a glass plate or similar surface from which it can conveniently be removed after drying. N ' I--To develop familiarity with the subjective evaluations thaf'j; follow; it is good practicelo make films of known resin composition by; applying control paints to glass plates or similar surfaces from which;- they can be readily removed after drying. 5. Pyrolysis 5.1 Summary of Test Method--A sample of coating:! placed in a small- test tube is burned over a hot flame. Thei way the coating burns and the odor and other characteristics of the- fume generated are recorded. The Beilstein test identifies the presence of chlorinated and other halogens. In coatings, chlorine-containing material is most often encoun-. tcred. For coatings not containing halogens, the odor is* recorded. . 5.2 Apparatus: 5.2.1 Flame. Source, including butane or propane utility torch. (Lighters do not provide a hot enough flame.) 5.2.2 Test Tubes--A suitable size is 10 by 75 mm (disposable culture tubes). 5.2.3 Copper Wire--A length of single-strand 16 to 18 gauge. AWG copper electrical wire, stripped of insulation sufficiently far that melted insulation cannot interfere with the test, is satisfactory. Leave about 6 in. of insulation as a heat insulator or provide a wrapping or handle for protection from heat. 5.2.4 Lead Acetate Paper. 5.2.5 Test Tube Clamp. 5.3 Procedure: 5.3.1 Put a small specimen of coating, preferably of one 906 ex (i DUP050298086 # 5043 TABLE 1 Classification of Coatings Frequently Used Basic Class Examples drying or baking (oxidizing) paint gnd enamel quer (drying by solvent evaporation) -x (drying by evaporation of water) Ically curing single package and ulti-comporient coating Iganic bellaneous unmodified drying oil oleoresinous (oil-modified, aikyd, epoxy ester, phenolic and other resins) vinyl (po!y(vinyl chloride-vinyl acetate)) poly(vlnyl butyral) chlorinated rubber styrene-butadiene rubber and similar rubbers bituminous (coat tar, asphalt) cellulose nitrate poiy(vinyl acetate) acrylic styrenated acrylic epoxy bituminous epoxy urethane polyester silicates and cement flame^sprayed silicones 'ce, in the test tube and hold the tube briefly in the hot e. Limit flame contact to the end of the test tube nediately around the specimen. As the specimen begins burn, observe the nature of deterioration and identify ting type as follows: Observation Identification -Fjange hvshapc; possible change in color, Continued heating causes sample to glow red |d deterioration, almost explosive in nature img cellulose nitrate, or similar some vinyl-type coatings N' 2--Melting, bubbling, and charring are common with most generic types and not definitive. 5.3.2 Continue heating until fume (smoke) fills the test tube. Most fumes are white or near-white; slight condensa tion of a clear liquid on the upper test tube wall is sometimes observed. Other observations and identifications include: Observation Identification Dark fume; clear brown liquid condensate Very dark, possibly sooty fume; dark condensate possibly epoxy bituminous N' 3--Bituminous coatings may be asphalt, coal tar, or combina tions. The test is not definitive. N' 4--Silicone coatings will form an ash upon pyrolysis at SOO'C. Such temperatures are outside the scope of this test. 5.3.3 Beilstein Test--Conduct the Beilstein test by first heating the bare copper wire in the flame until no color is imparted to the flame. Insert the heated wire into hot fume in the test tube briefly (1 to 2 s). Withdraw the copper wire from the test tube and immediately hold it in the flame again. Observe the flame over the copper wire for color and make identifications as follows: Observation No color Traces of green color Strong green color Identification no chlorine or chloride (or other halogen) content chloride contaminants from environment or minor component of coating chlorinated resin or chlorinated resin modifier With practice, the intensity of the green flame can be used to determine whether the chlorine containing component is major or minor. 5.3.3.1 Example 1--A very intense, relatively long-lasting repeatable green flame indicates chlorinated rubber or vinyl coating. NEGATIVE BEILSTEIN VERY UEAKIY POSITIVE STRONGLY POSITIVE ,f>ly odor" "Bu-rn-iIng hair" "Swee1t" or "Swee1t or" od. o[.r nondesc| riptive vnionnedgeasryc"ripotrive Sooty, tarry smoke acrid odor `.isfoluble Solvents Nat soluble in solvents Bdirsesaokslveusp oinr ethanol Mineral Spirits i e.tive for i;p|aonxdy afyteivseterfor Negeapatnoivdxey for Laacterxy,licin,cludes positive -for polyester apscctooeymltryaeb<tnievne)ian-,btyioulntasdiene, resinous inr)igJl-ico,il Keepppaucoolktxxiayy-cgoooenrrepbspoioi.nntxugeynlneierttsotuesr Polyester Solu1 ble Asp alt Not s1 oluble XyleIne Solui ble Coal1 ter ______1 Acetone1 Soak- 1 DiMsocinroimlnooaral tion Asp1thalt discSoevloerreation | Coal tar Includes both emulsion and solvent-borne coatings Mineral Spirits Soluble Not soluble Lacqi uer, Xyleine ssttyyrrieennnceleu--bdauicntragydlaietnee, _____I arondsinssimilar resins Soluble Nrofcoosot rilnsosorrilguoohbrlltle) Chlalrocurqbinubaeetrresd JMI8K --> soluTbr1 ulelty Viniyl copolymer (lacquer) sSolliugbhletl.y psoesvseirbele swelling wi thout upobnresaokaukping Modifiedi vinyls FIG. 1 Suggested Test Row Chart for Coatings Identification 907 S') I DUP050298087 # 05043 5.3.3.2 Example 2--An intense or moderately intense relatively short-lived green flame, which may or may not be repeated, indicates chlorinated plasticizer in a nonchlorinated resin binder. N' 5--Although fluorinated resins also give a positive Beilstein test, they are less likely to be encountered in industrial applications than chlorinated resins. N ' 6--If the sample includes hydrated nraterial, for example, concrete or plaster, water will be liberated by burning and will condense on the wall of the test tube. Halogen liberated from the paint will be absorbed into the condensate. The copper wire must be brought into contact with the condensate to avoid a false negative. N' 7---Those experienced with the Beilstein test may prefer to run it on a specimen not subjected to pyrolysis. 5.3.4 Odor Test--Conduct the odor test only if the Beilstein test is negative (no green flame). N' 8: Warning--Hot chlorine or fluorine-containing fumes are. extremely irritating and potentially hazardous. Tip the test tube so that the fumes flow toward the open end of the tube. Gently wave a hand over the mouth of the test tube and carefully smell the odor of the fumes as they dissipate from the mouth of the test tube. Avoid overexposure to the fumes. 5.3.4.1 Indications are subjective, but the following classes can be assigned: Observation Identification Oily oleoresinous Very sweet acrylic latex Vinegary; acetic acid poly(vinyl acetate) Burning hair epoxy, epoxy ester, bituminous epoxy Burning rubber polysulfide No strong odor inorganic, cementitious Acrid (biting) odor, with bituminous sooty or tarry smoke 5.3.5 Use the lead acetate paper to verify the presence of a sulfide component by holding a piece of moistened lead acetate paper over or in the mouth of the test tube. A sulfur-containing component is present if the paper rapidly darkens. 6. Solubility Tests 6.1 Chemically cured, inorganic, and aged oleoresinous coatings are not resoluble in the solvents originally used in producing the coatings. Lacquers and some latex coatings are resoluble and the strength of the solvent required to cause the coating to dissolve can be used to classify the coating. 6.2 Reagents--Solvents used, listed in order of increasing power of solvency (that is, ability to dissolve a resin), are as follows: 6.2.1 Denatured Ethanol (Ethyl Alcohol): 6.2.2 Mineral Spirits (Petroleum Spirits)--Aliphatic hy drocarbon solvent with typical Kauri-Butanol value (KB) of 25 to 45. 6.2.3 Xylene (Xylol)--Aromatic hydrocarbon solvent with typical KB of 98. 6.2.4 Methyl Isobutyl Ketone (MIBK, 4-Methyl-2- Pentanone). 6.2.5 Acetone (Dimethyl Ketone, 2-Propanone). 6.3 Procedure: 6.3.1 Although a stirring rod or a gloved finger-tip can be used, the test is best done by a finger-rub technique on the coating film itself. The sensations perceptible by touch are valuable in interpreting results. Alternatively, the solubility tests may be done by soaking portions ofthe film insolvents, in which case porcelain spot plates and glass stirring rods can be used. N' 9: Warning--These solvents can cause skin irritatio; L..( dermatitis, Minimize time of contact of solvents with skin and discon tinue use if irritation occurs. 6.3.2 Finger-Rub Test--Beginning with ethanol, dampen a fingertip and.rub the surface of the film briskly in a circular motion 5 to 10 mm (`A to V2 in.) in diameter. Renew the test solvent frequently as required. Continue rubbing at least 30 s or until definite effects are observed. Continue with each solvent in increasing power of solvency by cleaning the fingertip in each succeeding solvent before using that test solvent and selecting a new spot on the film or an untested chip of paint for each solvent used. No t e 10---If the coating film on the test surface is chalky, the first fxnger-rub test done with ethanol will liberate much of the chalk, which will dry quickly on the finger as a powder. Repeating the test will reveal much less or no color and the test surface will appear unchanged. If a chalk is liberated, iise ethanol to clean the test spot for subsequent solvent tests. 6.3.3 Solvent-Soak. Test--The full series of solvents can bq .XN-rE |'3b<iare I Wiriv , SoiffereJ njn concurrently. Place five chips in a spot plate dish ,Lnd pour a small amount of each solvent over one of the chips. Periodically stir the solvent and rub the chip with a stirring rod until definite changes occur. Add additional solvent, if necessary due to evaporation, and observe extent of discolor ation of the solvent and whether the chip softens, breads apart, swells, dissolves, or a combination thereof. Note whether a color, different from the color of the topcoat is imparted to the solvent, indicating dissolution of an interme diate or primer coat. If portions of the chip dissolve or SrfoTi IU| CO Ifr-.NpTi '^rafcutmre discolor the solvent, soak up the solvent with a paper towel and add fresh solvent if undissolved chip remains. If no further effect occurs, wash the remainder of the chip b\ gentle swirling, soak up the solvent, allow the chip to dr)', and proceed with pyrolysis or other tests. :fil N' 11: Precaution--Do not attempt to bum a solvent-wet chip ojr'i heat solvent in a test tube, as the liquid may suddenly boil, possibly ;; causing burns or loss of specimen. 6.3.4 Observe the effects of rubbing or soaking and classify as follows (the results for the soaking test are more difficult to interpret than for the finger-rub test): 6.3.4.1 No effect or small amount of color transfer to the fingertip or rod (due to chalk or film surface abrasion while rubbing). 6.3.4.2 Softening of the film, with resin rolling into small balls under the fingertip or rod. 6.3.4.3 True solubility with film dissolving, becoming sticky, and transferring in relatively large liquified quantity to the fingertip or rod. 6.3.5 Succeeding layers in a coating system may be individually tested if they are visually different; for example, colored topcoat, white or grey intermediate coat, and brown or red primer coat. To test visually different layers, repeat edly rub the spot with an effective solvent and wipe away dissolved coating periodically until a sublayer of different color is clean, then continue the test with the effective solvent on the sublayer. If that solvent is ineffective, repeat the test on the same spot with the next stronger solvent in the series. If that solvent is effective, repeat the test on a new P.5 908 DUP050298088 D 5043 ods cj UorM* i' 1lame circuit theajj asi 30%' *J| 'li cajJr tteVK hat test ''*'1 fcen or area, and when the sublayer is uncovered, allow gpivent to evaporate, then test the coating with the St solvent in the series, continuing up the series until lity is again observed. If a sublayer of coating is not by any solvent in the series, that layer may be |ted and collected by chipping or scraping for a sis test. || Interpretation ofResults: |i No Effect with Any Solvent--.Chemically cured, ed (aged) oleoresinous, or inorganic. p 12--With prolonged contact, oleoresinous coatings may soften Inkle. Absence of wrinkling, however, is riot indicative of absence iifesinous coatings. H'-' Fire;, i 3 k^fSTTM iBm&L angegl 41* > van i I. ull-Mj ;.ctyPVH stirring \cnh;tE& iscoJ6i * brea^.fti I. Note,,-] iti'rrap^W ohc bol r tovl't TJ? * *W :lnp tq Hi P Breaks Up or Dissolves in Ethanol---Latex coating iMvinyl butyral). fed3--Latex coatings are normally not soluble in mineral spirits IliPnly slightly affected in the short time of the test by xylene and ^(resulting in surface slickness). Ethanol will not dissolve any Ipmrnon coating type in this test, but it may affect considerable ipriisfer from weathered epoxy films. Bituminous emulsions do [gak up or dissolve in ethanol. J3 Dissolves in Mineral Spirits--Asphalt coatings and ger coatings other than chlorinated rubber and vinyls. Jptible resins include styrene-butadiene, styrenegte, and similar resins, but do not include polymers neoprene which are not normally used in solvent gon coatings. J' 14--Lacquer coatings other than chlorinated rubber and vinyl fcntain chlorinated plasticizers that give a positive Beilstein test, gp ,15--Some coal tar coatings strongly discolor mineral spirits || not significantly dissolved by the solvent, |4 Dissolves in Xylene but Not in Mineral Spirits-- ctar coatings and chlorinated rubber-based coatings, piently associated with solution of a chlorinated rubber pis the ability of the resin to "string" between surface of ilm and finger when the finger is pulled away from the :t (.hip; ng anj d>l..*, t mortal rw*!u n nju% -jp 0 sntaiC |t5 Dissolves in MIBK but Not in Xylene--Poly(vinyI fde-vinyl acetate) solution coatings. |TE 16--Vinyls may soften with resultant "resin roll" in the Jffhib test with xylene. Some vinyls, modified with polymers such as |fhylene, may not readily dissolve in MIBK, but feel slick with | color transfer in the finger-rub test and may swell up to 2Vi times Ut dissolving in the MIBK soak test. They may also feel similarly With some color transfer in xylene. |' 17--Latex binders merely soften in the short time the test is jornifigy-l iuantir>$ nay be1, TM sample. 1 rberopwena.^t^ la a'1 [iffaeut fcjsc,. " , repeat'. it in thclgfl i a new' A It may be possible to further differentiate between Hit and coal tar coatings using acetone. Soak a chip of Sineus coating in a test tube of acetone for several ftffites. Agitate gently and observe for extent of discolora- | Asphalts only very slightly discolor acetone while coal strongly discolor it, but there can be intermediate |Ses of discoloration that do not permit discrimination. It : possible by simple methods to differentiate between a >l5fent-borne (cutback) and water-borne (emulsion) bitumi$us coating. lest for Polyester Coatings i This test identifies polyester-based coatings from the group of chemically cured coatings that are not affected by the solubility test. 7.2 Apparatus: 7.2.1 Test Tube. 7.2.2 Medicine Droppers. 7.3 Reagents: 7.3.1 Potassium Hydroxide in Methanol. 7.3.2 Hydroxylamine Hydrochloride Solution in Meth anol, 10 %. 7.3.3 Ferric Chloride Solution, saturated in distilled water. 7.3.4 Hydrochloric Acid, 3 %. : 7.3.5 Warm Water, 125F (50C). 7.4 Procedure--Place a small quantity of the film sample in a test tube. Add 10 drops of potassium hydroxide solution and 6 drops of hydroxylamine hydrochloride solution. Place the test tube in a container of warm water for 2 min. Add 10 drops of hydrochloric acid and one drop of ferric chloride solution. 7.5 Interpretation ofResults: Observation Muddy violet color Absence of color or light yellow color Identification dibasic polyester is present dibasic polyester is not present 8. Test for Epoxy Coatings 8.1 All common epoxy coatings give positive results in this test. Epoxy ester coatings may also give positive results. 8.2 Apparatus: 8.2.1 Ashless or Low-Ash Filter Paper, 90 to 110-mm diameter. 8.2.2 Medicine Droppers. 8.3 Reagent: 8.3.1 Sulfuric Acid, concentrated. 8.4 Procedure--Support the filter paper off surfaces that may be damaged or could cause interference in the test. A watch glass can be used to support the paper. Place a specimen of coating in the filter paper. Place 2 or 3 drops of sulfuric acid directly on the coating. Place 1 or 2 drops of acid elsewhere on the filter paper not in contact with the coating. Let stand for 1 to 2 min. Carefully hold and tilt the filter paper toward the vertical until the acid runs down the paper away from the specimen. Wait 10 to 30 s or until there is development of color in the acid itself, not on the coating. 8.5 Interpretation ofResults Observation Identification . Development of red to violet color in the acid presence of epoxy Absence of color in the add coating is not epoxy 8.5.1 If red to violet color develops in the drop of acid not in contact with the specimen, then the paper is contaminated or was placed on an epoxy or epoxy-coated surface. Discard and repeat the test. A very slight pink color may develop in the acid. This is not a positive result. Bitumen-filled epoxies may discolor the acid enough to mask color development If the acid stream is discolored brown to black, carefully rinse the filter paper briefly in water or under running water if available. Color from a positive test will remain in the filter paper after the discoloration is washed off. The filter paper itself will be charred brown by the acid and eventually dissolve. The color of a positive test should occur early enough to be seen before the paper chars. 909 irii DUP050298089 # D 5043 9. Test for Pigments that Contain Lead and Hexavaient Chromium 9.1 Summary of Test Method: 9.1.1 Knowledge of the presence of pigments that contian lead and hexavaient chromium in an existing coating system may be important in a decision on whether the coating system is to be retained and recoated or on the method of removal and disposal of the coating system residue. 9.1.2 Pigments that contain lead or hexavaient chro mium, or both, may be used both in primers as rust- inhibitive pigments and in topcoats as weatherrresistant colored pigments. Depending on the ease with which a coating system can be separated, topcoats and primer coats may be individually tested for lead or hexavaient chromium, or both. 9.1.3 The presence of lead and hexavaient chromium containing pigments can be qualitatively determined in the field with the following two tests. Both tests can be done directly on the coated surface or on chips or dust of the coating placed in the well of a spot plate. 9.2 Apparatus--Glass beakers, jars or bottles, porcelain spot plates, sandpaper, razor blade or knife. 9.3 Reagents: 9.3.1 Sodium Sulfide Powder or Crystals. 9.3.2 Hydrochloric Acid, concentrated. 9.3.3 Diphenylcarbohydrazide Powder. 9.3.4 Phosphoric Acid, concentrated (85 %), 9.3.5 Acetone. 9.3.6 Denatured Ethanol. 9.3.7 Distilled or Deionized Water. 9.4 Preparation of Test Solutions: 9.4.1 A solution of sodium sulfide in water is used to test for presence of lead. Prepare the solution by dissolving 1.5 g of sodium sulfide in 20 mL of distilled wattjr and adding hydrochloric acid dropwise while swirling the solqtjon until a white precipitate forms and remains with continued swirling (pH should be about 8). A proportionally smaller or larger amount of solution can be made up, The solution loses strength with age. Test the solution by placing a drop on a strip of lead acetate paper and. observing the paper for the development of the black color of lead sulfide. If color development does hot occur, discard the solution and make a fresh one. ` 9.4:2 A solution of 1,5-dipheijylcarbohydrazide is used to test for the presence of hexavaient chromium. Prepare the solution using the following or proportionally smaller amounts of ingredients. Dissolve 0.5 g of 1,5- diphenylcarbohydfazide in a mixture Of 20 mL acetone and 20 mL ethanol in a beaker, warming the beaker in warm water if necessary to facilitate solution. Carefully add 20 mL of phosphoric acid to 20 mL of cold distilled Water in a separate container. Slowly add the acetone-ethanol mixture to the dilute acid solution and mix thoroughly by swirling. The 1,5-diphenyIcarbohydrazide solution is not stable. It may be stored for short periods of time in an opaque glass bottle but is best prepared just prior to use. The solution can be tested by placing a drop on a material known to contain a hexavaient chromium pigment. If a blue to violet color does not rapidly develop in the drop of solution, discard V solution and .prepare a fresh solution. 9.5 Procedure: 9.5.1 Abrade two separate spots on the coating film with sandpaper or knife if the tests are to be done on the coatii g surface. Alternatively, abrade one spot of the coating and collect the dust and flakes in two wells of a spot plate. Abrasion of the film is required to expose pigments in an aged, weathered film. 9.5.2 On one abraded spot or on the specimen in one well of the spot plate, place 1 or 2 drops of sodium sulfide solution. Development of a black or dark grey color on tin film or flakes indicates the presence of lead. Lack of color development indicates less than 0.1 % by weight lead (ap proximate practical limit of sensitivity of this test procedure). 9.5.3 Metals other than lead give a positive sulfide test bi; may 'not be common to coatings or usually do not interfere in this test in the form present. If there is doubt, laboratory'f testing beyond the scope of this test method isrequired ta; ' confirm the presence of lead: 9:5.4 On one abraded spot or to the second well of 1 spot plate place 1 or 2 drops of 1,5 diphenylcarbohydrazid solution. Rapid development of blue to violet color in tie solution droplets indicates the presence of hexavaient chro- " niium. r 9.6 Interpretation ofResults--The /combination of results; from the two tests, together with consideration of the color ot the coating, may be 'used to establish more definitely the'' pigments that are present, as shown in the following scheme, which is not all inclusive: Observation Positive for lead, negative for chromium Negative for lead, positive for chromium Positive for lead, positive for chromium 10. Precision and Bias Identification - - pigment is red lead, white lead, or : lead subside (while) ^:V pigment is zinc or strontium rhiom^* (yellow) chrome yellow, chrome green, chromes: orange, or molybdate grange (alt; 1 color pigments containing lead chromate) or basic lead silichromate (orange-red inhibitlve * pigment) H| 10.1 Precision cannot be determined for these methods because the variability of coatings on a surface doi3 not permit the collection of reliably uniform samples and', because few specimens will be tested from one partiralu coating. 10.2 Bias cannot be established 'for these test methods" because accepted reference standards are not available. 11. Keywords 11.1 coatings; field; generic resin; identification 910 DUP050298090 D 5043 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard aro expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn, your comments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. H you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 911 DUP050298091 Designation: D 5062 - 90f Standard Test Method for Resin Solution Dilutability1 This standard is issued under the fixed designation D 5062; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. tl N ' --Keywords were added editorially in March 1991. 1. Scope 1.1 This test method covers a titrametric/gravimetric determination of resin solution dilutability which gives a numerical value for the overall solubility of the resin expressed as percent dilutability. 1.2 This test method is applicable only if the test solution is of sufficient clarity to allow accurate visual judgement of the end point and of low enough viscosity for efficient mixing to take place. 1.3 This test method is primarily for, but not limited to, resins used in the printing ink industry. 1.4 The percent solvent tolerance of a resin can be determined using this test method if the solvent in the resin solution and the dilution solvent are the same. 1.5 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 1725 Test Method for Viscosity of Resin Solutions2 E 1 Specification for ASTM Thermometers3 3. Terminology 3.1 Definition of Term Specific to This Standard: 3.1.1 resin solution dilutability.--the maximum amount of diluent tolerated to reach a defined degree of turbidity; beyond this point, resin precipitation will occur. 4. Summary of Test Method 4.1 A sample of resin solution is weighed into a glass beaker that is'placed over a piece of 10 point print (standard newspaper print). 4.2 The dilution solvent is added slowly from a buret until the newsprint can no longer be read (cloud point) when viewed from the top of the beaker. 4.3 The percent dilutability is calculated by weight 1 This test method is under the jurisdiction of ASTM Committee D1 on Paint and Related Coalings and Materials and is the direct responsibility of Subcom mittee D0L37 on Ink Vehicles. Current edition approved May 25. 1990. Published July 1990. 2 Annual Book ofASTM Standards, Vol 06.02. 3 Annual Book ofASTM Standards, Voi 14.03. 5. Significance and Use 5.1 This test method provides a means for resin producers and users as well as solvent and varnish manufacturers t> rate various types of resins for solubility by assigning r numerical dilutability value. This percent dilutability value can be used to differentiate resin types for end users and can be utilized as a quality control tool by resin manufacturers 5.2 When running a series of these tests the same lot or batch of dilution solvent must be used throughout to ensure reproducible results. 6. Apparatus 6.1 Glass Beaker, 150-mL (51-mm diameter, 79-rrn height). 6.2 Graduated Buret, 50 mL. 6.3 Constant Temperature Water Bath at 25"C. 6.4 Thermometer, 0 to 40"C range with subdivisions of, 0.5*C conforming to Specification E 1. 6.5 Magnetic Stirring Bar and Stirring Plate or Stiirif, Bod. 6.6 Sheet of Newsprint, with 10-point (Note), No. 31^ old-style type, lower case letters 1.5-mm high with normal' spacing, upper and lower case with no italicized or bold letters. . N ' --The term point is derived from the American Point Systejn. ,, 72 points -- 1 in. 7. Reagents and Materials 7.1 Resin Solution--A resin solution prepared in such a way as to provide an accurate percent solids and to have sufficient clarity to allow accurate visual judgment of `he cloud point. The solution must also have low eno'ij||| viscosity at 25C to allow efficient mixing during the.^ addition of the dilution solvent. 7.2 Dilution Solvent--The dilution solvent for this test is i typically, but not limited to, a hydrocarbon. The dilution solvent should have minimal loss by evaporation at roam temperature. 8. Procedure 8.1 Preparation ofResin Solution: 8.1.1 The resin solution may be prepared by eitieri heating the resin/solvent combination as described in T( G Method D 1725, or dispersing using a high-speed mixer sui' as a blender. Please note results may vary dependent on method of preparation. 8.1.2 The ratio of resin to solvent in the preparaUi>" should correspond as much as possible to the intended end 912 J ( aid S5S3SSS85555 DUP050298092 D 5062 [if, use of the material, but should be chosen to avoid difficulty effecting solution at a low enough viscosity for efficient M mixing during dilution. `^8.1.3 The precision of weighing the resin and solvent (Should ensure a maximum deviation of 1 % in the desired ^concentration. This percent solids must not be altered during ifjC'im solution preparation by solvent loss. 8.2 Weigh a 150-mL glass beaker with the magnetic stirrer fir or stirring rod. Record this tare weight as Wt. m 5.3 Accurately weigh 10 0.1 g of the resin solution into ithe beaker. Record this sample weight as W2. ;y,|8.4 Place the .beaker in a 25`>C constant temperature bath j^ntil the resin solution reaches 25 PC as measured witji ife thermometer specified in 6.4. ; t 8.5 Prepare the dilution solvent by bringing it to a 'j?jflentperature of 25 PC before adding it tp the buret. 1C 8i6 Place the beaker over the piece of 10-point print and Kpgin adding solvent slowly (5 to 6 mL/min) while stirring. SfoiStire that the sample temperature remains at 25 PC, _ hich may require periodic return of the beaker to the Water jbatfi. If the sample has started to form' a haze it should not be ;^Tctjrned to the water bath. 8.7 Observe the 10-point print from the top of the beaker |>king through the solution. 8.8 If the resin solution begins to cloud, a'dd `solvent [pwly one drop at a time while continuing to mix. Do not jturn the sample to the water bath at this point. If more fan 100 g is required, the resin solution can be considered [finitely soluble unless otherwise specified in an agreement ftween the purchaser and supplier. 8.9 The end point is reached when the 10-point print rtannot be read looking through the solution from the top of beaker. |i;8.10 Record the final weight of the beaker and its contents fe). p.U Record the sample temperature at the end point. if iS;, Calculation j|9.1 Calculate the percent resin solution dilutability, D, as Plows: wi-(W, + D-- x 100 (0 9.2 Calculate the percent solvent tolerance of the resin, S, (percent resin solids at cloud point) as follows: IW, x (5/100)] T ------------------------------=-------x 100 W2 + IW,-(W, + W2)) (2) where S = resin in solution, %. 10. Report 10.1 Report the following information: 10.1.1 The identification of the resins and the solvent in the solution as well as the dilution solvent, 10.1.2 The method used to prepare the resin solution, 10.1.3 The percent solids of the resin solution, and 10.1.4 The percent resin dilutability value and operating conditions including air temperature, relative humidity, initial resin solution temperature, final resin solution tem perature, initial dilution solvent temperature, and final dilution solvent temperature. 11. Precision 11.1 An interlaboratory study was conducted in which one operator in each of eight laboratories determined the percent dilutability of two common resin solutions and two dilution solvents completed in duplicate on two different days. The pooled within-laboratory standard deviation was found to be 3.25 % of the value measured with 12 df. The between-laboratory standard deviation was 7.63 % of the value measured with 28 df. Based on these standard devia tions, the following criteria should be used for judging the acceptability of results at the 95 % confidence level. 11.2 Repeatability--Two results, each the mean of dupli cate determinations, obtained by the same operator should be considered suspect if they differ by more than 9.19 % of the value measured. 11.3 Reproducibility--Two results, each the mean of duplicate determinations obtained by operators in different laboratories, should be considered suspect if they differ by more than 23.38 % of the value measured. 12. Keywords 12.1 dilutability value; percent dilutability; printing ink resins; resins; resin solution cloud point; resin solution dilutability; solvent tolerance The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee andmust be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of`this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 913 DUP0502 98093 Designation: D 5063 - 90 Standard Guide for Use of Certification of Coating Conformance Form1 This standard is issued under the fixed designation D 5063; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the yearoflast reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This certification of coating conformance form pro vides procurement information concerning products being furnished in accordance with a specific coating specification and additional requirements contained in the purchase order (see Fig. 1). 1.2 The completed form can be utilized to help evaluate the acceptability of the paint being furnished. 2. Referenced Documents 2.1 ASTM Standards: D 16 Terminology Relating to Paint, Varnish, Lacquer, and Related Products2 1 This guide is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.45 on Marine Coatings. Current edition approved May 25, 1990. Published July 1990. 2 Annual Book ofASTM Standards, Vol 06.01. 3. Instructions for Completing Certification Form 3.1 Use only known and industry accepted descriptions. Standard definitions of terms relating to paint, varnish; lacquer, and related materials are provided in Terminology D 16 (see Fig. 2). 3.2 The sections are self-explanatory. Applicable informa tion in Section II should be provided by the buyer. Appli cable information in Section III should be provided by the seller. 3.3 For two-component coatings, separate forms should be provided for each component, if appropriate. 4. Keywords 4.1 certification form; conformance form 914 DUP050298094  D 5063 CERTIFICATION OF COATING CONFORMANCE FORM ^GENERAL TYPE AND DESCRIPTION: Generic Type: Manufacturer's Designation: Specification Number: Formula Number: Number of Components: Component Identification (if applicable): Color: ^ BUYER INFORMATION: Name ancf Address: Number: Date: CERTIFICATION OF CONFORMANCE FORM L GENERAL TYPE AND DESCRIPTION: Number: A001 Date: 6/26/88 Generic Type: Manufacturer's Designation: Specification Number: Formula Number: Number of Components: Component Identification: Color: Polyamide Epoxy Perfect Paint 1234 M1L-P-2444! Formula 150 Two Component A Green II. BUYER INFORMATION: Name and Address: American Shipbuilders 1234 Easy St. Anytown, USA Purchase Order Number: Release Number (if applicable): Part Number (if applicable): Item Number (if applicable): Stock Number (if applicable): j SELLER INFORMATION: I* Name and Address: Purchase Order Number: Release Number (if applicable): Part Number (if applicable): Item Number (if applicable): Stock Number (if applicable): III. SELLER INFORMATION: Name and Address: 0001-0002 #1 118 #3 4321 Perfect Paint Co. 11 Profit St. Paint City. USA Seller s Representative: (Indude Telephone Number) Batch Number. Lot No.: Date of Manufacture: Date of Expiration of Certification: ^ CERTIFICATION: This is to certify that the above material being furnished has been manufacid in accordance whh the specification and meets all specification requirements pained in the above purchase order. ft ft f NAME AND TITLE SIGNATURE FIG. 1 Certification Form Seller's Representative: (Include Telephone Number) Batch Number: Lot Number Date of Manufacture: Date of Expiration of Certification: IV. CERTIFICATION: i.B, Responsive 703/123-4567 88-F-01 ` 0001 6/20/88 6/19/89 This is to certify that the above material being furnished has been manufac tured In accordance with the specification and meets ail specification requirements contained In the above purchase order. l.M. Xpert, Tech Director NAME AND TITLE SIGNATURE FIG. 2 Example of Completed Form ' 6/26/88 DATE The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapprbved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 915 DUP050298095 Designation: D 5064 - 90 Standard Practice for Conducting a Patch Test to Assess Coating Compatibility1 2 This standard is issued under the fixed designation D 5064; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice covers the procedures for testing coating compatibility when maintenance of an in-place coating system is being contemplated. It does not cover procedures for assessing the integrity of the existing coating to determine if it can be repainted, nor does it establish the compatibility of the maintenance coating system with the substrate or corrosion products. The practice is intended for use in the field. N' 1--Pass-Fail Criteria (for example, adhesion requirements) are not established by this practice. These should be established by the user or specifier with input from the supplier. 1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2. i ASTM Standards: D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 D3359 Test Methods for Measuring Adhesion by Tape Test2 D4138 Test Method of Measurement of Dry Film Thick ness of Protective Coating Systems by Destructive Means2 D4414 Practice for Measurement of Wet Film Thickness by Notch Gages2 3. Terminology 3.1 Definitions--For definitions of terms used in this practice, refer to the Federation of Societies for Coatings Technology (FSCT) Paint/Coatings Dictionary.3 4. Summary of Test Method 4.1 The materials under test are applied to the previously painted surface after proper surface preparation. After the appropriate time has elapsed, the test patch is examined for 1 This practice is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee ,, DO 1.46 on Industrial Protective Coatings. Current edition approved May 25, 1990. Published July 1990. 2 Annual Book ofASTM Standards, Vol 06.01. y Paint/Coatings Dictionary, Federation of Societies for Coatings Technology, Philadelphia, PA, 1978. visual defects and adhesion is determined. 5. Significance and Use 5.1 In performing maintenance of a coating system, the new coating being applied must be compatible with the existing coating. While general guides exist which indicate compatibility of different generic types of coatings, differ ences in manufacturer's formulation and the condition ofthe in-place coating will affect compatibility. 6. Procedure 6.1 Select test locations for evaluation that properly char acterize differences in configuration of the structure and exposure, that is, vertical versus horizontal surfaces and bold versus sheltered exposure. A minimum of three test locations with one test patch in each is recommended. 6.2 The size of each test patch will be determined by the size and configuration of the test locations. Each test patch shall be as large as possible, with a minimum size of 10 ft2 (0.93 m2) recommended. 6.3 Clean the surface of the test areas using the methods specified for the maintenance painting procedure (Note 2). Alternative methods of preparation may also be evaluated in separate, adjacent tests. N' 2--This test method assesses compatibility with the existing coating only and does not apply to areas where the substrate is exposed by the methods of preparation. 6.4 Measure the existing coating thickness in accordance with Test Methods D 1186, D 1400, or D 4138, as appro priate for the substrate. 6.5 Measure the ambient conditions and surface temper ature and assure the conditions are within the limits specified by the coatings manufacturer for the product being tested. 6.6 Apply the test coating to the thickness recommended for the particular job. Use the application technique as intended for use on the full-scale job. If agreed upon between the purchaser and the seller, the method of coating applica tion may be different from that used on the job, that is, brush application of the test patch even though spray application will be used on the job. However, this can cause some error and is not generally recommended. 6.7 Immediately after application, measure the wet-film thickness in accordance with Practice D 4414. Make correc tions to the application, if necessary, by either applying more material if the expected dry-film thickness is low or applying another test patch if the expected dry-film thickness is above the recommended maximum. Inspect each patch for appli cation defects such as runs, sags, and holidays. If such defects cannot be corrected as a part of the initial application process, prepare a new test patch. 6.8 After the coating has dried, measure the dry-film ! j \ | \ I [ fjiicknt at P 4 NOTE thanes the aver 6.9 Cure c L-ong-t cotnpa evalua 6.9J possibl should 6.9.1 imum 6.1C patch cracki 916 DUP0502 98096 D 5064 thickness in accordance with Test Method D 1186, D 1400, or D 4138. N' 3--When using Test Methods D 1186 or D 1400, the dry film sickness is the difference in average thickness of the coating system less the average thickness of the in-place coating. 6.9 Allow the coating to cure or weather prior to testing. Cure durations are defined as long term and short term. Long-term curing provides the most reliable assessment of compatibility. Short-term curing provides for more rapid evaluation of results. 6.9.1 Long-Term Curing--Curing for as long a time as possible, with a minimum of six months preferred. Curing should span seasonal weather changes. 6.9.2 Short-Term Curing--Curing at the following min imum times based on average daily (24 h) temperatures: 50`F(10"C) 70F (21"C) 90`F (32`C) 14 days 10 days 7 days 6.10 After curing, examine the total surface of each test patch for wrinkling, blistering, mudcracking, checking, cracking, peeling, lifting, and disbonding. Measure or rate the adhesion in a minimum of five locations per test patch in accordance with Test Methods D 3359. 6.11 Examine the test patches for the defects noted in 6.10 on a regular schedule, discounting rust caused by previous tests such as adhesion measurements and destructive film thickness measurements. 7. Report 7.1 Report the following information: 7.1.1 The identity of the structure tested, the location and size of the test patches, the identity of the test coating, the method and grade of surface preparation, and the method of coating application. 7.1.2 For each test patch, the dry film thickness measure ments and average of the in-place coating, the dry film thickness measurements and average of the test coating, the elapsed time for each evaluation, the visual defects noticed, and the results of adhesion tests. 8. Keywords 8.1 coating; coating compatibility; coating test patch; paint; paint compatibility; test patch The American Society far Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement or such rights, ere entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feeI that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 19T6 Race St., Philadelphia, PA 19103. 917 DUP050298097 Designation: D 5085 - 90 Standard Guide for Assessing the Condition of Aged Coatings on Steel Surfaces1 This standard is issued under the fixed designation D 5065: the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A,number in parentheses indicates the year of last reapproval. A superscript epsilon (r) indicates an editorial change since the last revision or reapproval. I. Scope 1.1 This guide provides general guidelines for a detailed assessment of the condition of aged coatings on steel structures and the extent of rust breakthrough of the coated surface. Additional assessment may be required to support coating failureanalyses-or othef job specific needs. 1.2 This guide does hot address the problem of deter mining the structural condition of a steel substrate. It provides procedures to determine the percent of the surface rusted, but not the severity, condition, or cause of such rusting. N' 1--A more comprehensive condition assessment procedure, Practice F 1133, based upon two sets of visual standards, one for level and one for exteht of deteriorationv'has been developed for determining the condition of coatings on ship hulls. 1.3 This standard does not purport to address the safety problems associated with its use. It i,s,the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory Imitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D610 Test Methods for Evaluating Degree of Rusting on Painted Steel Surfaces2 D 660 Test Method for Evaluating Degree of Checking of Exterior Paints2 D714 Test Method for Evaluating Degree of Blistering of Paints2 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D3359 Test Method for Measuring Adhesion by Tape Test2 D 4214 Test Methods for Evaluating Degree ofChalking of Exterior Paint Films2 D4541 Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers2 D 5043 Test Methods for Field Identification of Coatings2 F 1133 Practice for Inspecting the Coating System of a Ship's Underwater Hull and Boottop During Drydocking3 1 This guide is under the jurisdiction of ASTM Commitlee D-l on Painl and Related Coalings and Materials and is the direct responsibility of Subcommittee DO 1.46 on Industrial Protective Coatings. Current edition approved May 25, 1990. Published July 1990. 2 Annual Book ofASTM Standards, Vol 06.01. 3 Annual Book ofASTM Standards, Vol 01.07. 2.2 Steel Structures Painting Council Standard:4 SSPC-PA-2 Measurement of Dry Paint Thickness v , Magnetic Gages 3. Summary of Practice 3.1 This practice for assessing the condition of coatings! consists of identifying general types of components of ai structure and assessing each separately for commonly occur^ ring modes of coating deterioration and rust breakthrough ofi the coating using visual standards and simple evaluiioi* tools. A form for recording the results of die assessr, fq procedure (Fig. 1) is provided. 4. Significance and Use 4.1 Assessment of the condition of aged coated suit; strengthens decisions on when coating maintenance :s quirpd, aids in the selection ofeffective coating maintenance! procedures, and provides a means to characterize perionranee of coating systems. 5. Procedure 5.1 Survey the structure to (2) determine the general t of unique components (for example, for fuel tanks components may be shell, roof, ladders, and piping) and dw service exposure environment for each, (2) visually identify I areas having a typical level of coating deterioration and ru't ] breakthrough for each component and (i) identify areasJ having a much greater visual level of deterioration thaiil typical and unique environmental conditions that may j correspond to these areas (for example, bridge expansion' joints). Record a description of the components and their? general environment on an inspection form and describe areas having greater deterioration, as well as any unique^ associated environments in the remarks column. A suggesfod> general format for data collection is shown in Fin. i Modification of the form (for example, adding or dele specific items) will be required for each specific application. 5.2 Based upon the knowledge of what constitutes typ 11 1 deterioration for each component as determined in the iniiiu! survey, examine the condition of the coating on a represeit|j tative sample of each component. Rate the condition of the?| coatings using the appropriate ASTM visual standard for riistj breakthrough (Test Methods D 610), blistering (Test Methqdiil D 714), peeling (use Test Methods D 610 to report amount), chalking (Test Methods D42I4), and cracking/checkift$j (Test Method D 660) of the coating film. Record the rating in the appropriate column of the report form for each ` Available from Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, ;i PA 15213. 9.18 j Rra ApplEd refel DUP050298098 Original Coating Sysiem rface Preparation Applied -------- Description Local Environ ment 0 5065 Condition Assessment Inspector . 1 st Maintenance Coating System Surface Preparation Year Applied _____ Primer Midcoal _________ Midcoat _________ Topcoat _________ Ratings Under film . n. .. Condition* Peelns Blistering Cracking . Overall Environment 2nd Maintenance Coating System Surface Preparation Year Applied ______ Primer ___________ Midcoat __________ Midcoat __________ Topcoat _________ Measurements Chalking Thickness = Adhesion Rusting corresponds to Test Methods D 610, that is, that observed upon visual inspection of the n under an intact coating as'described in Section 4. " FIG. 1, Example 1 Report Form surface while underfilm condition corresponds to substrate ponent. Determine and record the type of peeling, for mple, intercoat delamination. Rate the condition in ugh areas to ensure that for each component the coating ation,iis representative of the condition over, the entire qture. If additional areas of greater deterioration are :ted during this assessment, make note of them fn the arks column. . OTE 2--For the purport of an initial general assessment, cracking checking'can be assessed as one type of failure, using the pictorial ards in Test Method D 660 to define type and extent. . ' s When rusting beneath an intact coating, film is susexamine the condition of the underlying substrate. Ove apparently indfiSt coatings using chemical strippers closely spaced parallel- knife cuts. For structural-'steel, ~ine the type of previous surface preparation from the nee of millscale or profile. Identify evidence of corron from the presence of pits, black anodic spots or ion scale, or from results of a test for ferrous iori vising ium ferriferrocyanide paper. Record the results of the rnation on the report form. 5.4 Using one of the procedures described in Test ods D 1186, determine the coating thickness in enough of each component to ensure a representative measure, rd the measured thicknesses. 5.5 Using one of the procedures described in Test Methods D 3359 or D 4541, determine coating adhesion in enough areas of each component to ensure s representative measure. Record the adhesion reading and the type of procedure and equipment used. N' 3--The number of areas in which coating thickness and adhesion is measured will depend upon the desired precision of the measurement. More measurements would be made on structures in which precise knowledge of the thickness, and adhesion of the coating is required. SSPC-PA-2 states the required number of thickness measure ments as a function of coating area for conformance of thickness-to a specification. 5.6 If required for a maintenance decision, identify the generic type(s) of the existing coating film component from records or using the procedure in Test Method D 5043. To the extent possible, each layer of the film should be charac terized. 6. Report 6.1 Prepare an inspection report. Figure 1 provides an example of the tyiies of information to be included. 7. Keywords 7.1 assessment; coatings; condition; field; paint; weath ered . The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in. this standard. Users of this,standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprovedor withdrawn, your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend it you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. 1916 Race St, Philadelphia, PA 19103. 919 DUP0502 98099 Designation: D 5066 - 91 Standard Test Method for petermination of the Transfer Efficiency Under Production Conditions for Spray Application of Automotive Paints-- Weight Basis1 This standard is issued under the fixed designation D 5066; the number immediately following the designation indicates ihe year of original adoption or. in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 3.1.2 transfer efficiency--the ratio of the weight of paint 1.1 This test method provides procedures for determina solids deposited to the total weight of paint solids used M:1s!-l' tion of the transfer efficiency (using a weight method) under during the application process, expressed as a percent. production conditions for in-plant spray application of 3.1.3 paint weight solids content--the weight of the non automotive paints. volatile materials in the liquid paint material divided by the 1.2 The transfer efficiency is calculated from the weight of total weight of the paint, times 100, determined by Te the paint solids sprayed and that deposited on the painted Method D 2369. part. The recommended approach involves painting the part 3.1.4 paint density--the mass of a unit volume of the directly. Also described is an alternative approach for liquid paint material at any given temperature, determined painting parts covered with aluminum foil. by Test Method D 1475. 1.3 This standard does not purport to address all of the 3.1.5 satellitepaint supply system--a smaller, paint-circu safety problems, if any, associated with its use. It is the lating system separate from the main production paint- responsibility ofthe user of this standard to establish appro circulating supply system capable of supplying paint under priate safety and health practices and determine the applica the'same conditions. bility of regulatory limitations prior to use. Specific hazard statements are given in 10.9. 4. Summary of Test Method 4.1 The weight of the part to be painted is determined 2. Referenced Documents 2.1 ASTM Standards: D 1475 Test Method for Density of Paint, Varnish, Lac quer, and Related Products2 D 2369 Test Methods for Volatile Content of Coatings2 2.2 USEPA/MVMA (Motor Vehicle Manufacturers Asso ciation) Standards: EPA 450/3-88-018, U.S. Environmental Protection before and after the paint application process. The weight of liquid paint used per part is determined from material usifr. and part processing records. The determined weight sclids content of the paint material is determined and used to1, calculate the paint solids sprayed per part. The transfer efficiency of the process is calculated by dividing the weight of paint solids deposited by the weight of the paint solids sprayed. Agency Protocol for Determining the Daily Volatile Organic Compound Emission Rate of Automobile and Light Duty Truck Topeoat Operations,3 EPA Federal Reference Method 24--Determination of Volatile Matter Content, Water Content, Density, Volume Solids, and Weight Solids, of Surface Coatings4 5. Significance and Use 5.1 This test method is specifically directed at the spuj r painting of automobile car and light duty truck bodies, i general principles are applicable to the painting of othn , automotive parts. . 5.2 This test method may also be used to measure transfer 3. Terminology efficiency in full-sized painting facilities simulating prodUution conditions and operations. 3.1 Descriptions of Terms Specific to This Standard: 3.1.1 paint--the liquid material that is applied onto the 6. Interferences part to cover or coat the surfaces. 6.1 Limitations include the ability of the weighing device to determine accurately the weight of the paint solids 1 This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.55 oa Factory Applied Coatings on Preformed Products. Current edition approved May 15, 1991. Published July 1991. Originally deposited on the part and the capability ofaccurate measure ment of the amount of paint sprayed (see Section 7). 6.2 It may be difficult to cover the surface of complex shaped parts with aluminum foil (see 11.6.11). published as D 5066 - 90. Last previous edition D 5066 - 90. 2 Annual Book ofASTM Standards, Vol 06.01. * Available from Superintendent of Documents, U.S. Government Printing 7. Apparatus Office. Washington, DC 20402. Refer to EPA 450/3-88-018 dated December 1988. This protocol makes reference to the determination of production spray transfer efficiency. 4 Available from Superintendent of Documents. U.S. Government Printing Office, Washington, DC 20402. Refer to CFR 40, Part 60, Appendix A. 7.1 Tension Load Cells, with upper/lower transition pieces. 7.1.1 1500-lb (682 kg) capacity with 0.05-lb (0.02 kg) precision for weighing automobile body and support franc 920 DUP0502981OO Q) D 5066 |?rl.2 500 to 800-lb (227 to 364-kg) capacity with 0.05-lb 02 kg) precision for weighing mix tanks or automobile iinponents. number of vehicles or. parts .(see> 9,1.U. : r; ^ <r . 9.1.1 At least 5.0 lb (2.27 kg) of paint ^material must be used during the test with the specified weighing equipment. jjg.1.3 A safety cable is required for upper to lower transi- 9.2 Before a satellite paint supply system can berijsexfeit fe. must be demonstrated that the system is capable of supplying m Electronic Digilizer/Readout, readability of 0.05 lb the paint at sufficient volume and pressure to maintain m2 kg) and special Filtering. normal process conditions (fluid deliveries of the spray ^7:2.1 The electronic digitizer/readout shall meet OIML devices) and that the paint can be maintained at a represen Iternational Organization of Legalized Metrology) tative temperature and viscosity for the duration of the test jjeificatidiis.5 period. These requirements can best be assured by mounting [7.3 Voltage Regulator. the satellite tank on a load cell or scale and directly piping it f.A Swivel Devices, as required. into the production supply system ofthe spraybooth. For this (f.5 Rule and Calipers for measuring diameter of paint procedure the requirements are as follows: jlply tank shaft, etc. 9.2.1 Level and calibrate,a weighing device (see Section 7) If.6 Sample Containers, clean and airtight for paint mate- for weighing the satellite supply tank. 9.2.2 If an electronic weighing device is used, it must be ||.7 Lifting Device and Support Frame Apparatus to lift turned on long enough to achieve stability,: following the 3y. manufacturer's directions. All weighing devices must be (7.7.1 Total weight must not exceed capacity of load cell or situated to minimize disturbance from vibration or air ale. movement. Ifr.8 Standard Calibration Weight, approximately 2 lb (0.9 9.2.3 Introduce the paint material, reduced to spraying viscosity, into the tank to be weighed. Before the test is |7.9 Measure Stick, Statist precision spring' tempered, conducted, be certain that fluid flows are properly set, that all i chrome finish, 36 in. (91.4 cm), with 4R graduatiohs, or supply and return lines are filled with the paint, and that no jiiivalent. leaks are present in the piping system. 9.2.4 Shut off the agitator to minimize vibration during [Paint Usage Measurement Procedures the weighing of the system. y e jr ir- 18.1 Transfer efficiency measurement requires that accu- i measurements be made ofthe quantity of paint material ed in the application process during the time period ociated with the coating of specific vehicles or parts. Two neral procedures are applicable for accurately measuring fit usage. 18.1.1 The preferred procedure is to determine the weight paint used during the application study period. Under pical production conditions, such weighing may be diffijlt, due to the large number of applicators requiring paint iipply from a common tank. If a separate, isolated paint apply tank is used in the test; it is important to control paint cosity, temperature, and flow rate consistent with the liar production system (see 9.1). 8.1.2 Where direct paint usage measurement by weight is at practical, an alternative procedure for determining paint ge by volume is suggested. This procedure involves asuring the drop in paint level in the paint supply tank 9.2.5 Calibrate the weighing device in accordance with manufacturer's instructions. Weigh and tare a lifting frame, if used to support the satellite paint supply tank. 9.2.6 Weigh the satellite paint supply tank before the test vehicles or parts are run. Flexible connections are required to minimize strain. Carefully note the configuration of the tank so that the same configuration is used for both initial and the final.weighing (that isvhose connections, height, etc.). Weigh the tank until 2 consecutive measurements are obtained within the measurement error of the weighing system 0.05 lb (0.02 kg). Average the two readings. The satellite tank may be left on the weighing device during the painting operation to monitor painting usage on a continuous basis. 9.2.7; After painting the test vehicles or parts, reweigh the satellite paint supply tank in accordance with 9.2.5 and 9.2.6. 9.2.8 Obtain representative paint samples immediately after completion of the test for solids and density analysis. during the test. To provide sufficient accuracy, it may he pessary to paint a "block" (isolated group) of similar \ chicles or parts from the paint supply system while usage 10. Paint Usage Determination by Tank Level Measurement (Volume Procedure) measurements are taken. Typically, this may require 10.1 This procedure for determining the paint usage 5e punting approximately 30 vehicles (see 9.2). requires that the drop in the liquid level in the system supply is tank be measured accurately. This procedure is applicable e- Paint Usage Determination by Weight Procedure with either a satellite system or a main-mix room supply 9.1 This procedure for determining paint usage during the Safest is preferred when a satellite paint supply system is ' ailable for the process to be tested. With this procedure, it ! usually easier to isolate paint usage for measurement ^purposes, and accurate results can be obtained with a smaller system. A sufficient number of parts must be processed in the test block to provide at least a 3-in. (7.6-cm) drop in the liquid level in the paint supply tank. Careful measurement is critical to the overall accuracy of the transfer efficiency test. This procedure consists of the following: 10.1.1 Accurately measure the inside diameter of the paint supply tank(s) to be used for the various test materials. Electronic digitizer. Model 5322, available from Sterling Scale Co., 20950 Bocoirigi Southfield. Ml 48075, has been found suitable for this purpose. If the agitator shafts, fill pipes, or any other objects are located in the measurement zone, the occupied volume of 921 DUP050298101 5066 these items must be determined and subtracted from the total volume. Careful selection of the section of the tank for the test measurement will minimize the difficulty of this task. The measurements are used to develop a conversion factor between level drop and volume of paint. 10.1.2 Most main paint supply systems consist of two tanks connected together to maintain the material supply. During the test, the paint supply tank must be isolated. Check to ensure that there is no leakage or overflow between the two tanks and that the directional valves for paint return function properly. Make sure that these checks are made just prior to and after the test, and are done by measuring the volume in both tanks. 10.1.3 Place the test paint, which has been reduced to spraying viscosity, into the paint supply tank to be measured. No material additions or reductions may be made to the tank during the test. Before the test is conducted, make certain that valving is set so that paint is being drawn from the test tank and returned to the test tank, and that all air has been removed from the delivery system. 10.1.4 With satellite paint supply tank systems, special care must be taken to ensure that all fluid lines are completely filled. 10.1.5 Prior to taking the volume measurement, turn off any agitation within the tank that will interfere with the measuring process and then turn it back on after the measurement. 10.1.6 Record the tank levels before and after the test. Take the initial reading just prior to the first test vehicle or part of the block that enters the first application station in the tested process. Take the final reading just after the last vehicle or part has left the last application area in the tested process. 10.1.7 With clearcoat (or other paint materials that cannot be isolated to a specific block of cars due to other connected operations such as repair), take the initial reading as the first vehicle or part in the test block enters the first station applying clearcoat. Take the final reading when the vehicle after the last job in the test block enters the first station, applying clearcoat (the same point at which the initial reading was taken). If this is not done, the block size for clearcoat will be different from the block size for basecoat (this is acceptable but must be accurately reflected in the calculations). 10.1.8 The measurements are to be taken to the nearest '/i6 in. with a measuring stick with Vis-in. (!.6-mm) or less graduations. Measurements are made from the top of the tank to the top of the liquid level at least 3 to 4 in. (7.6 to 10.2 cm) from the sides of the tank. The top of the tank is to be determined by laying a straight edge across the top of the tank in the same position for each measurement. N' --Caution--Any measuring instruments used in this procedure must be effectively grounded before contacting the coating tank or coating liquid surface. Review all measuring instruments for suitability and resistance to the paint solvents prior to the test. 10.1.9 It may be necessary to provide two-way radio communication between the mix-room monitor and the tested process operation to coordinate the measurement process and timing. 10.1.10 Obtain representative paint samples immediately after completion ofthe test for density and solids determin tions. 11. Paint Solids Deposited Measurement Procedure 11.1 To determine the transfer efficiency, it is necessary determine both the weight of paint solids sprayed per vehii or part and the weight of paint solids actually deposited on the object in the tested process. These are obtained weighing vehicles or parts incorporated in the same sairmfi (block) used to obtain the paint usage measurement. * 11.2 Vehicle or Pan Weighing Procedure--The weight paint solids deposited during 'the application proo-j determined by weighing the vehicle(s) or part(s) prior to and after the paint is applied and baked. At least two vehicles o parts are required to be tested. A control part is also run j.* weighed before and after the application process. No painr applied to the control part in the process. The control required to determine weight loss from miscellaneous matef rials (primarily sealants and plastics applied prior to the tested process) that may occur in the drying oven. I difference in the weight of the measurement vehicles justed for the weight loss in the control vehicle or part, is weight of paint solids applied in the tested process. 11.3 Weighing of the parts requires the use of a precision weighing device and digitizer as described in 7.1 and 1 ' \ lifting frame and hoist are required to support the test vehicle. The measurement site(s) must be selected to avoid disturbance caused by air movement or production activities and to allow convenient removal of the test vehicles or parts from the production line and their subsequent replacement to the production line. Fork trucks or other mechanical handling aids along with sufficient manpower to move file vehicle bodies into and out of the weighing frame will bef required. 11.3.1 Passenger car bodies generally will weigh 800 to, 900 lb (364 to 409 kg). Since the maximum capacity of the' specified load cell is 1500 lb (682 kg), the weight of the lifting frame and rigging must be kept to less than 600 lb (273 kg) or a higher capacity load cell with the specified accuracy must be utilized. 11.4 It is critical that the vehicles or parts be allowed to cool completely to room temperature prior to weighing. Closely monitor heavy-metal sections (usually around the! door frames) as these areas will cool more slowly than.; exterior body surfaces. If during the weighing process there is any doubt that the vehicle or part is fully cooled, weigh the test part and allow it to stand 15 to 20 min and weigh again! If a weight increase of more than 0.05 lb (0.02 kg) is noted, allow the body to cool an additional 15 to 20 min and repeat the weighing procedure. Repeat this process until consistent weights are obtained. 11.5 Check that all accessories and miscellaneous mate rials (hangers, spacers, etc.) remain in the' same position (either on or off) for both the initial and final weighings. 11.6 Weighing Procedure: 11.6.1 Turn on the weighing device and digitizer and allow them to warm up in accordance with the manufactur er's instructions. 11.6.2 Zero the instrument in accordance with manufac turer's instructions. 11.6.3 Attach the lifting frame to the load cell. Lift and 922 : DUP050298102 5066 Ithe frame until two consecutive readings within 0.05 m kg) are obtained. Record this tare weight, W,. J|4 Mount a completely cooled vehicle or part into the icediire * is nece yed peT', deposit^ 5 obtair i same"! enicii* The weif, n prociglf S) PI ..| !,, wo (luin s also rutff SS. \( 'he .,ir lancjic. i pnnr t, ig ovenJL t vehicles'! orPart,M cess of a pre^| 1 ILUj 7 2- . pon iht cted to If tion actw| tides orcg repUvc r meebsS to mom i| rame v. ill Jframe. Lift the test unit until it is completely clear of xrier and fully suspended by the load cell. If the test Res not hang level, adjust the suspension point on the Tfframe and recheck for.proper tare weight. If necessary, Ilibration weights may be used to help level the test Kjbut be certain to include this weight in the initial L jfp Allow the suspended vehicle or part to completely fee (usually 2 to 3 min). Be certain that nothing is ling the test unit or suspension frame and record the 5.6 Add a standard calibration weight to the suspended Be or part and check for instrument accuracy, jgbrate the system if a discrepancy is noted. P>.6.1 Select the calibration weight to represent the fated increase in weight of the vehicle or' part in the j|ng process. Jji>,7 Lower the vehicle or part back onto the carrier to lye the weight from the load cell. Relift the vehicle or land weigh as just indicated until two consecutive fits within 0.05 lb (0.02 kg) are obtained. Record the ge of two consecutive initial weights, that is Wx for part nd Wcj for the control. 16.8 Remove the first body and repeat 11.6.5 through 1;7 for the other vehicles and the weight loss control fee (if included in this test run). Between test measurets and after the last unit is weighed, resuspend the empty ft frame and verify the tare weight, Wv I,6.9 Apply the paint to the specified vehicles or parts, j|ing the control unit to proceed through the spraybooth bven uncoated. veigh ipacity I of the'i '.b (2731 :curacyii 1.6.9.1Considerable care must be taken in handling the bed units to eliminate any weight gain or loss due to ifiling, parts addition, parts removal, or miscellaneous Ks. II.6.10 After the vehicles or parts have been painted and Id in the oven, allow them to cool to room temperature e allow to weighing! around slowly tha. ocessthen > d, weigh thJjjj weigh agaitifl kg) is notedjg n and rq |t to reweighing. Repeat the weighing procedure in 1. through 11..6.8 and record the weights, Wlf for the Red part (1) and WcJ for the control. p.6.11 Foiled Part Procedure--The procedure is iden- ; to that described in 11.2 except that aluminum foil is Applied to the vehicle or part. All the surfaces to be hted are covered with foil as smoothly and tightly as |?ible to ensure that the covered surface is representative he area painted in the normal production environment. il consistetfl Measurement of Other Paint Usage reous mate- 2.1 When the measurement of paint used cannot be com- me positionj Jtely isolated to the application process under test because of eighings. Ee process and facilities arrangement, it may be necessary to Stain an estimate of paint solids deposited from the same igitizer and1' Tmt supply system in the nonisolated operations (such as nanuface .J |)air, etc.). With this estimated value, the total paint solids |posited in the main process can be directly correlated to the h manufac-j rtount of paint used in calculating the resultant transfer |ciency. Such a correlation can be established by either ill. Lift and ] king a separate estimate or measurement of the paint used or the paint solids deposited outside the tested process. The amount of material involved should be small (less than 5 %} relative to the total paint used or deposited. 12.2 While an estimate of paint used is generally pre ferred, in practice it is usually easier to obtain an estimate of the amount of paint solids deposited onto the test unit. For repair type operations, an estimate of paint solids applied may be obtained by counting the number of panels repaired while the test block is being processed and multiplying by the square feet per panel and the average film build applied (determined from measurements or historical data). This technique works well since almost all repairs involve com plete body panels for which data can readily be obtained. 13. Analysis of Paint Samples 13.1 Make the following analytical determinations for each paint sample obtained: 13.1.1 Weight Fraction Solids, in accordance with Test Method D 2369 per EPA Federal Reference Method 24. 13.1.2 Paint Density, in accordance with Test Method D 1475. 13.2 These determinations are required to calculate transfer efficiency. Obtain separate determinations for each paint material used in each test. 14. Calculations and Report Submission 14.1 Upon completion of the test and receipt of the paint analytical results, the transfer efficiency calculations can be made in accordance with the following procedure: 14.2 Calculate the average weight gain of the vehicle or part, corrected for the weight gain or loss of the control unit. Sum[ Wf - W,] -IKs- Wc,\ (1) where: Gavg = average weight gain, lb (kg), W = weight, lb (kg), Wr = final weight, lb (kg), W{ - initial weight, lb (kg), n - number of test unitscoated, c = control, Wc_p = final weight of control vehicle or part, lb (kg), and Wc i = initial weight of control vehicle or parts, lb (kg). 1*4.3 Calculate the average amount of paint used during the test period by either the weight procedure or the volume procedure. 14.3.1 Weight Procedure (see Section 9): P,,s = IP> - PrVm (2) where: Pavg = average weight of paint used during the test, lb (kg), Pj = initial weight, lb (kg), Pr = final weight, lb (kg), and m -- number of units measured. 14.3.2 Volume Procedure (see Section 10): (3) where: V = volume of paint used during the test, D = paint density in accordance with Test Method D 1475, and m = number of units measured. 923 J | r DUP0502981 03 # D 5066 14.4 Calculate the average paint solids used during the test period. 6*avg = ^avg x F (4) where: Szvg = average weight of paint solids used during the test, lb (kg), and F = weight fraction solids in the paint material from Test Method D 2369. 14.5 Calculate the transfer efficiency T result. r= Cavg/Savg X 100 (5) 15. Precision and Bias 15.1 Precision--Engineering estimates based on error' sumptions indicate an accuracy of 5 % can be expected fH typical automotive painting operations. ,ur' 15.2 Bias--Since there is no accepted reference procedhJ suitable for determining the bias for this test method statement on bias is being made. ' 16. Keywords 16.1 automotive painting; production method; soia' plied; transfer efficiency- TM The American Society for Testing arid Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or for additional standards and shouid be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7916 Race SI, Philadelphia, PA 19103. A 924 wjspw-.r DUP050298104 Standard Specification for Artists' Watercolor Paints1 This standard is issued under the fixed designation D 5067; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the iasl revision or reapproval. CI N' --Table XI.1 was editorially corrected in March 1991. Number of one phthalocyanine blue pigment is 74160. fs specification establishes requirements for compoysical properties, performance, and labeling of jtercolor paints. |s specification covers pigments, vehicles, and addiftiirements are included for pigment identification, ss, and consistency. 3.1.3 Appearance terms used in this standard are defined in Terminology E 284. 3.2 Descriptions ofTerms Specific to this Standard: 3.2.1 watercolor paint--a pigment dispersion in a water soluble gum/resin vehicle that dries water soluble and is intended primarily for transparent applications. fble 1 lists some pigments meeting the lightfastness ents in this specification. In order to identify other s that meet these requirements, instructions are r test specimen preparation. Test methods for ting relative lightfastness are referenced. 4. Significance and Use 4.1 This specification establishes quality requirements and provides a basis for common understanding among producers, distributors, and users. 4.2 It is not intended that all paints meeting the require enced Documents ?TM Standards: Test Methods for Coarse Particles in Pigments, tes, and Paints2 ments be identical nor of uniform excellence in all respects. Variations in manufacture, not covered by this specification, may cause some artists to prefer one brand over another, either of which may be acceptable under this specification. 0 Test Method for Fineness of Dispersion of Pig- 5. Labeling Requirements nt-Vehicle Systems2 6 Practice for Labeling Art Materials for Chronic faith Hazards2 p3 Test Methods for Lightfastness of Pigments Used ^Artists' Paints2 84 Terminology of Appearance of Materials3 5.1 Pigment(s) Identification: 5.1.1 Every label shall include for each pigment contained in the paint (/) the information underlined in Table 1 (which includes the Common Name, Colour Index Name, and any additional terms necessary to identify the form of the pigment) and (2) the appropriate Lightfastness Category. 'nology 5.1.2 The complete pigment identification given in Table 1, which also includes the Colour Index Number and a efinitions: simple chemical description, shall be given in an appropriate ,1 Colour Index Name--consists of the category (type producer publication. Manufacturers are encouraged to put or pigment), general hue, and an assigned number this complete identification on the container label when label to a colorant in the Colour Index4 as an international size permits. "cation system. 5.1.3 The Common Name shall be placed on the front of ,1.1 Discussion--For example, the Colour Index the label and shall be the name of the paint except as of one phthalocyanine blue pigment is Pigment Blue described in 5.1.5 and 5.1.6. Other identification may be 15>. placed elsewhere on the container. s.2 Colour Index Number--a five-digit number given in 5.1.4 The Colour Index Name may be spelled out in full 1 olour Index that describes the chemical constitution of or abbreviated depending on the size of the label. Example: orant. Pigment Blue 15, or Pig. Blue 15 or PB 15. .2.1 Discussion--For example, the Colour Index* * 5.1.5 Substituted Pigments--In the case of substituted pigments, the word "Hue" in equal size letters shall follow in the title, on the front ofthe tube, immediately after the name his specification is under the jurisdiction ofASTM Committee D-1 on Paint /elated Coatings and Materials and is the direct responsibility oF Subcom' D0I.57 on Artist Paints and Related Materials. " em edition approved May 25, 1990. Published September 1990. of the pigment that has been simulated. Directly below the title, the Common Name of the significant pigment used shall be given in letters no less than the next type size smaller ,/inuat Book, ofASTM Standards, Vol 06.01. *nmial Book ofASTM Standards, Vol 14.02. . olour Index, 3rd ed., The Society of Dyers and Colourists, London, than the title. For example: COBALT BLUE HUE p75, five vols and revisions. Available from the American Association of Chemists and Colorists, PO Box 12215. Research Triangle Park, NC (ULTRAMARINE BLUE). 5.1.6 Proprietary names or optional names may be used 925 DUP05 0298105 # D 5067 TABLE 1 Suitable Pigments List N' --Underlined information and the lightfastness category in the table shall be included on every label. Key: Ugptfastness Category: Lighlfastness f Excellent Lightfastness Lightfastness II Very Good Lightfastness Abbreviations Used for Cofour Index Names; NR Natural Red PB Pigment Blue PBk Pigment Black PBr Pigment Brown PG Pigment Green PO Pigment Orange PR Pigment Red PV Pigment Violet PW Pigment White PY Pigment Yellow Pigment Notations: (CC) Concentrated cadmium pigments may contain up to 15 % barium sulfate for color control. Cadmium-barium pigments contain a much higher amount of bdnu m sulfate. 1 *** * (NA) Colour Index name or number not assigned. (SM) Sensitive to moisture in direct sunlight. Colour Index , Name Lightfastness Category Watercolors Common Name and Chemical Cla: Colour index 3 Number . PO 20 PO 20:1 PO 62 PR 101 PR 101 PR IQt PR 101 PR 101 PR 104 PR 108 PR 108:1 YELLOWS Arylide Yellow 10G, with option of adding,the name Hansa Yellow Light, arylide yellow Barium Chromate Lemon, barium chromate Chrome Yellow Lemon, lead chromate and lead sulfate Cadmium Yellow Light, concentrated cadmium zinc sulfide (CC) (SM) Cadmium-Barium Yellow Light, cadmium zinc sulfide coprecipitated with barium sulfate (SM) Cadmium Yellow Medium or Deep, concentrated cadmium suffide (CC) (SM) Cadmium-Barium Yellow Medium or Deep, cadmium sulfide coprecipitated with barium sulfate (SM) Aureoiin, with option of adding the name Cobalt Yellow, potassium cobaltinrtrite Mars Yellow, with option of adding the name Yellow Iron Oxide, synthetic hydrated iron oxide Mars Orange, synthetic hydrated iron oxide Yellow Ochre, natural hydrated iron oxide Arylide Yellow FGL. arylide yellow ORANGES 11710 77103 77600 77205 77205:1 77199 77199:1 77357 77492 77492 77492 11767 Cadmium Orange, concentrated cadmium sulfo-selenide (CC) Cadmium-Barium Orange, cadmium sutfo-selenide coprecipitated with barium sulfate Benzimidazolone Orange H5G, monoacetotone REDS 77202 77202:1 NA fij Indian Red, synthetic red iron oxide (bluish hue) tight or English Red Oxide, synthetic red Iron oxide (yellowish hue) Mars Red, with option of adding the name Red Iron Oxide, synthetic red iron oxide Mars Violet, with option of adding the name Violet Iron Oxide, synthetic iron oxide (violet hue) Venetian Red, synthetic iron oxide (yellowish hue) Chrome Orange, lead chromate and lead molybdate Cadmium. Red Light, Medium, or Deep, concentrated cadmium-selerio sulfide (CC) Cadmium-Barium Red. Light, Medium, or Deep, cadmium seleno-sulfide coprecipitated with barium sulfate 77491 77491 77015 7749.1 77605 '77202:1 77202:1 PURPLES Cobalt Violet, cobait phosphate, cobalt ammonium phosphate Ultramarine Red, complex silicate of sodium and aluminum with sulfur Ultramarine Violet, complex silicate of sodium and aluminum with sulfur Manganese Violet, manganese ammonium pyrophosphate Quinacridooe Violet, quinacridone violet b 77360 77362 77007 77007 77742 73900 BLUES II* Phthatocyanine Blue, copper phthalocyanine Prussian Blue, with the option of adding the name Milori Blue, fsrriammonium ferrocyanide Cobalt Blue, oxides cf cobalt and aluminum 74160 77510 77346 Ultramarine Blue, complex silicate of sodium and aluminum with sulfur Manganese Blue, barium manganate with barium sulfate Cerulean Blue, oxides of cobalt.and tin 77007 .77112 77368 Cerulean Blue, Chromium, oxides of cobalt and chromium 77343 GREENS Phthalocyanine Green, chlorinated copper phthalocyanine Chromium Oxide Green, anhydrous chromium sesquioxide Viridian, hydrous chromium sesquioxide Cobalt Green, oxides of cobalt and zinc 74260 77288 77289 77335 926 jig:. 1n1. * m. > '> M : ->I, 4ord;. ub|; s .. Iff- DUP0502981 06 D 5067 ' * Sr 7 Lightness Category Watercoiors TABLE 1 Continued Common Name and Chemicald Class BROWNS Burnt Sienna, calcined natural iron oxide Burnt Umber, calcined natural iron oxide containing manganese Raw Sjenna, natural iron oxide Raw Umber, natural iron oxide containing manganese BLACKS Lamp Black, nearly pure amorphous carbon Carbon Black, nearly pure amorphous carbon Ivory Black, amorphous carbon produced by charring animal bones Gray Hydrated Aluminum Silicate, hydrated afuminum silicate WHITES I Zinc White, zinc oxide with option of adding the name Chinese White jpiese pigments were put into the lightfastness II category pending results of retesting. Colour Index NuttibiV ; 77492 77492 77492 77492 77266 77266 77267 77017 tided the Common Name(s) given in Table 1 appears on [front of the label directly under the proprietary or Inal name in letters no less than the next type size |er than the proprietary or optional name. |.7 Mixed Pigments--Artists' paints containing more Jr one colorant comply with this specification if all fred pigments used are on the suitable pigment list {Table lid provided the mixture itself has passed all other test lirements in this specification. The lightfastness category |] be that of the least lightfast pigment. This lightfastness flgory may be changed if these paints are tested for Itfastness in accordance with Test Methods D 4303 and gits indicating a different category are submitted to fM Subcommittee DO 1.57 for evaluation. 5.2 Provide on the label the identification of the gum/` |n used. 1.3 Lightfastness--The label shall contain the word Ightfastness" followed by the appropriate rating, I or II, as mn for each pigment in Table 1. J.3.I Lightfastness I pigments, when made into paint Jbimens as described in Section 7 and exposed, tested, and fed in accordance with Test Methods D 4303, shall have a fjjbr difference (AE*ab) of 4 or less CIELAB units between {specimens measured before and after exposure. 5.3.2 Lightfastness II pigments, when made into paint Kcimens as described in Section 7 and exposed, tested, and led in accordance with Test Methods D 4303, shall have a Jjor difference (AE*ab) of more than 4.0 but not more than 1 CIELAB units between the specimens measured before Id after exposure. 15.3.3 Pigments were placed in a lightfastness category' on ip basis of either known historical performance in art works $f the ratings from four lightfastness tests conducted as - llscribed in Test Methods D 4303. Results from further tests these, or other pigments, are solicited by Subcommittee 101.57. 5.3.3.1 The lightfastness category of a pigment shall be |hanged if results from several further tests conducted in ac cordance with Test Methods D 4303 and approved by ASTM S ibeommittee DO 1.57, establish a different lightfastness Category than the one given in Table 1. 5.3.3.2 Additional pigments shall be placed in Table 1 Ifler they have been tested for lightfastness in accordance with Test Methods D 4303 and the test results submitted to ASTM Subcommittee DO 1.57 for evaluation, provided the results demonstrate that the pigments have the lightfastness ratings required for Lightfastness I or Lightfastness II, as described above. 5.3.4 For information and to establish nomenclature, pigments in Lightfastness III category are given in Table Xl.l in Appendix XI, but are not to be used in paint conforming to this specification. These pigments have a color difference before and after exposure of more than 8.0 but not more than 16.0 CIELAB units. 5.4 Toxicity--All products and labeling must conform to the Federal Hazardous Substances Act and to Practice D 4236. 5.5 Statement of Conformance--"Conforms to ASTM Specification D 5067," or "Conforms to ASTM D 5067," or "Conforms to the quality requirements of ASTM D 5067." This statement may be combined with other conformance statements, siioh as, "Conforms to the quality and health requirements of ASTM Specification D 5067 and Practice D 4236." 5.6 Address--IncLude on the label (I) the name and address of the manufacturer or importer and (2) the country of manufacture. 6. Quality Assurance for Artists' Watercolor Paints 6.1 Conditions not Covered in This Specification That Affect Artists' Watercolor Paints: 6.1.1 Substrate--The effective pH of the paper used will affect the long-term color of the applied watercolor. 6.1.2 Environmental Conditions--Factors such as temper ature, humidity, airflow, and light conditions affect applica tion properties, drying time, and adhesion. 6.1.3 Storage--With aging and elevated temperatures there may be a change in consistency and a discernible separation of vehicle. 6.2 Vehicles--Only water soluble gums/resins shall be used. 6.3 Pigments--Pigments used in watercolors shall be limited to those in Table 1. Their lightfastness rating shall be the numeral given in the same row. 6.4 Additives--Thickeners, preservatives, surfactants, and humectants may be used to achieve consistency, prevent 927 DUP0502981 07 # D 5067 microbe deterioration, and control application results. 6.5 Inerts--Inerts shall only be used to produce desirable working qualities. 6.6 Preparation of Sample--For paste and fluid paints, empty the contents of the previously unopened container onto a glass slab and mix thoroughly with a spatula to a homogeneous sample. For cake paints, take a piece of the cake on a glass slab and add water and mix until a homogeneous paint is formed. 6.7 Coarse Particles--Faints shall be free of oversize particles and shall form a uniform film. The maximum content of coarse particles shall be 1 weight % as determined by Test Methods D 185. 6.8 Fineness of Dispersion--Determine the fineness of dispersion by Test Method D 1210. For paste paint, on a glass plate, using a spatula, mix the paint with an equal volume of water until homogeneous. The maximum allow able grind reading is 1.5 mils (40 gm). 6.9 Consistency--Paints shall be smooth and easily solubilized with water to a homogeneous color. 6.10 Freeze-Thaw Stability--Using a freezer that has a temperature of 20F (-7C) or lower, subject the paint to five freeze-thaw cycles. A freeze-thaw cycle shall consist of freezing the paint to a solid state (minimum of 18 h) and then thawing the paint to room temperature (minimum of 5 h). The paint shall then meet the requirements of 6.7, 6.8, and 6.9. 7. Lightfastness Determination 7.1 If a pigment is not listed in Table 1, test specimens of a watercolor containing the pigment shall be prepared. These test specimens shall be tested in accordance with the require ments for exposure and evaluation given in Test Methods D 4303. N ' --A report of the results of these tests may be submitted to Subcommittee DO 1.57 for inclusion of the pigments in Table 1. The report shall include information on test conditions and instruments used and shall be accompanied by the test specimens (which will be returned). 7.2 Materials: 7.2.1 Filter Paper, 15.0-cm diameter, ashless.5 7.2.2 Drawdown Bar with 3-mil (75-pm) aperture. 7.2.3 Posterboard, lightweight, approximately 20 mils (0.5 mm) thick, having a glossy finish on one side. 7.2.4 Distilled Water. 7.2.5 Acrylic Latex Adhesive. 7.3 Preparation of Test Paints: 7.3.1 The pigment to be tested may be milled in a soft 5 Whatman No. 42 Filter Paper, available from Fisher Scientific, 711 Forbes Ave,, Pittsburg, PA 15219, has been found satisfactory for this purpose. paste consistency. If a prepared artists' paint of known ' composition is available it may be used for this test instc. d preparing a standard. * 7.3.2 Dilute the watercolors with water and drawdown on paper until the spectrophotometric measurement of thedrai'u paint shows from 35 to 45 % reflectance at the wavelength maximum absorption for that pigment. The wavelength X * maximum absorption is located at the point of lowest ^ reflectance on the spectral curve between 420 and 620 nm If" using a tristimulus filter colorimeter, the lowest of the three filter readings is the region of maximum absorption and the ' dilution should be adjusted so that a reading of 35 to 45 % reflectance is obtained with this filter. The diffuse wh'- reference standard for all measurements should have an absolute reflectance between 97 and 100 %. 7.3.3 Use an applicator with a 3-mil (75-jj.m) aperture to make a drawdown on the filter paper. Tape the filter paper to'J a smooth surface such as a piece of glass. Place the .. drawdown bar just above the upper edge of the paper so it is 3 ready to use. Pour a small amount ofthe diluted paint, which is thoroughly mixed, onto the top of the filter paper. Using the drawdown bar, draw the paint down, running the excess offthe edge ofthe filter paper at the bottom. Quickly untape the filter paper and hang it to dry at room temperature. There will be a dark puddle area where the paint was originally applied, but the remaining part of the paper will be uniform in color for use in obtaining spectrophotomeli' measurements. 7.3.3.1 Prepare four specimen panels for each pigment under test. Two are used in the first lightfastness tests and, 1 two are retained in subdued light, one for visual comparisons with the exposed panels and one in case a third test is needed to supplement results from the first two tests, as described 11. Test Methods D 4303. 133.2 Apply the test paints to the filter paper as de scribed in 7.3.3. The panels should be air dried for 2 h and then put in an oven at 50C for overnight drying. 7.3.3.3 Cut the uniform color section of the filter paper drawdown panel into I '/2-in. (38-mm) square panels. Adhere the panels to the light posterboard (see 7.2.3) using a th coat of an acrylic-latex adhesive. The size of the posterboard shall conform to the dimensions of the exposure equipment test racks. 8. Exposure 8.1 Conduct exposure tests, calculate mean color difft ence, and assign pigments to lightfastness categories . s described in Test Methods D 4303. 9. Keywords 9.1 lightfastness; quality requirements; specimen prepara tion; watercolors iu 5. ;fast > i. T1-; rre--1| tNo\ }Ligl ) C0I1 olour |) Narni fJM 3112 as Edtorii! , N` ; r' - iv 928 M DUP050298108 # D 5067 APPENDIX (Nonmandatory Information) XI. LIGHTFASTNESS III I) The pigments in Table XI. 1 axe not sufficiently list to be used in paints that conform to this specifica- IThese pigments are listed here solely to establish common terminology. They may be satisfactory when used full strength (without dilution) or with extra protection from exposure to light. TABLE X1.1 Lightfastness 111 -Underlined informatton and the lightfastness category in the table shall be Included on every label. tNotatlans: ^btfast type |lir Index |iame Ini SfTlLFlt E12 iios WTa fT5a Lightfastness Category ,111 III 111 !H III til i corrected. Common Name and Chemical Class Arvlida Yellow G, with option of adding the name Hansa Yellow Medium, arylide yellow Arvlide Yellow 5GX, with option of adding Hansa Yellow 5GX, aryffde yellow Isoindotinone Yellow R, tetrachtorolsolndolinone Vermilion, mercuric sulfide Naphthol AS-D. napbthal AS*D Quinacridone Magenta, quinacrldone Colour Index Number 11680 11741 NA 77766 12370 73915 The American Society lor Testing and Materials takes no position respecting the validity of any patent rights asserted In connection with any item mentioned in this standard. Users of this standerd are expressly advised that determination ol the validity ot any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapprmed or withdrawn. Your comments are Invited either for revision of this standardor lor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. D U P0502 98109 Designation: D 5068 - 90 Standard Practice for Preparation of Paint Brushes for Evaluation1 This standard is issued under the fixed designating. ..D 5068;' the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval, A superscript epsilon (<) indicates an editorial change since the last revision or reapprpval. 1. Scope 1.1 This practice describes the preparation of paint brushes for evaluation. 1.2 This practice is applicable to paint brushes 2 to 4 in. (50 to 100 ntm) in width. 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Summary of Practice 2.1 Using a paint chosen for the evaluation, the brush to be tested is repeatedly loaded with this paint and brushed out over a specified area in a specified application time. 3. Significance and Use 3.1 Until a paint brush is fully wetted with paint, only part of the paintloaded onto the brush can be transferred to the surface being painted. By properly preparing the brush before using, the amount ofpaint delivered to the surface can be made more uniform and reflect real use. 4. Apparatus 4. ] Container, to hold paint, for example, a quart cati. 4.2 Test Brush, 2 to 4 in. (50 to 100 mm) in width. 5. Materials 5.1 Test Paint. 5.2 Brush-Out Panels, or other typical panels to be used.2 5.3 Masking Tape, to secure the panel to a flat surface. 1 This practice is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.6ton Paint Application Tools. Current Edition Approved May 25, 1990. Published July 1990. 2 Any smooth type panel, for example, upson boards, can be used. A Leneta 8H-BW Chart, available from The Leneta Co., P. O. Box 86, Ho-Ho-Kus, NJ 07427, has been found satisfactory for this purpose. 6. Procedure 6.1 Secure the brush-out panel with masking tape to a flat smooth, horizontal surface. 6.2 Dip the test brush into the specified paint to the depth! shown below: Brush Width, in. (mm) Depth, in. (mm> i 2 and 2 Vs (50.and 62.5) 3 and 3`A (75 and 87.5) 4(100) V/2 (38) m (45) 2(50) 6.3 Hold the brush at the specified depth in the paint for' I0.s. Remove and hold the brush vertically for 30 s allowing* any excess paint to drain, 6.4 After the drain period, immediately apply paint to tie. | specified initial area on the brush-out panel as indica below: Brush Width, in. (mm) Initial Area, cm2 2 and 2`A {50 and 62.5) .3 to 4 (75.to 100) 250 500 6.5 Application time shall be 15 s for 2 and 2V2-in. (5 and 62.5-mm) brushes and 20 s for 3 to 4-in. (75 to lOO-miu) brushes. 6.6 Repeat this.procedure three times, 6.7 Maintain the level of paint in the container. Keep the angle of the handle and displacement ofthe'filaments of Hr test brush uniform throughout the entire series. When applying paint, always displace the test brush filament abouf j one third to one half of the filament length and maintain lit? handle perpendicular to the paint-out surface. 6.8 When applying paint, always start in the middle of the,, area to be painted with each loading. This leaves-the excc.'. paint in the middle where it is easiest to spread to the area being covered and willTesult in a more uniform coverage (see Fig. 1). 7. Keyword 7.1 brush preparation > f. 930. DUP0502981 10 # D 5068 PAINTING FINISHING 250( 9 s FIG. 1 Paint Application The American Society for Testing'and hfatertote takes no position respecting the validity of any patent rights asserted in connection With any item mentioned in this standard. Users of this standardare expressly,advised that determination of the validity of <my suchpatent rights, and the risk of Infringement of such rights, are entlreiy their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and If not revised, either reapproved or withdrawn. Yourcomments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, ti you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP05029811 1 t Designation: D 5069 - 90 *j Standard Practice for Preparation of Paint-Roller Covers for Evaluation1 This standard is issued under the fixed designation D 5069; ihe number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last rcapproval A superscript epsilon (t) indicates an editorial change since the last revision or reapproval 1. Scope 1.1 This practice describes the preparation or breaking-in of paint-roller covers for evaluation. 1.2 This practice is applicable to paint-roller covers having nap lengths up to Vi in. (13 mm). 1.3 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Summary of Practice 2.1 Using the paint chosen for the evaluation, the paintroller cover to be tested is repeatedly and generously loaded with paint and painted out over the same area of approxi mately 4 to 6 ft (0.4 to 0.6 m2) until it is saturated with paint, that is, the paint-roller cover cannot pick up any more paint, nor apply any more paint to the area being used for break-in. 3. Significance and Use 3.1 Until a paint-roller cover is saturated with paint, only part of the paint loaded onto the paint-roller cover can be transferred to a surface being painted. The remainder of the paint is absorbed into the fabric of the paint-roller cover. The amount of paint absorbed by a paint-roller cover is inversely proportional to the amount already present within the paintroller cover. By saturation of the paint-roller cover before testing, quantitative inaccuracies of the amount of paint de livered to a surface are eliminated. 3.1.1 Using a saturated paint-roller cover enables the user to apply paint at controllable spreading rates. 3.1.2 Using a saturated paint-roller cover affords repro ducibility when repeating a test. 4. Apparatus 4.1 Paint Tray. 4.2 Paint Roller Frame, of the same size as the paint-roller cover being prepared. 5. Materials 5.1 Paint, to be used in test. 5.2 Primed or Painted Surface, to be used for the rollers cover break-in. 6. Procedure 6.1 Place the paint-roller cover on the frame. 6.2 Load the paint-roller cover with the paint from' tray by rolling the paint-roller cover over the surface oft paint so that just the nap is submersed. See Fig, 1. 6.3 Roll out the roller cover on the surface being used: break-in in an upward and downward motion in no larger, area than 2Tt. (0.6 m) high by the width of the roller cov.-r' 6.4 Reload the paint-roller cover with paint and roll oui in the same manner over the same area. Do not increase; area except as necessary to control excess dripping of pain 6.5 Repeat the above procedure as necessary until following conditions are met: 6.5.1 Reloading the paint-roller cover does not result in j increased paint pickup. 6-5.2 There is so much paint on the surface being used'! that the fully loaded paint-roller cover cannot transfer ; more paint to the surface. 6.5.3 When the above conditions are met, there will be much paint on the roller cover that constant movem< (turning over) is necessary to prevent dripping, and the pane will show profuse sagging of the paint. About six roller-cotei loadings are usually necessary to achieve this. 6.6 The roller cover is now prepared for immediate testing. 7. Keywords 7.1 break-in; paint roller; paint-roller cover; test.prepare*:! tion; roller m f m 1 This practice is under the jurisdiction of ASTM Committee D-J on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee D0L61 on Paint Application Tools. Current edition approved May 25, 1990. Published July 1990. FIG. 1 Loading the Paint Roller tfv. 932 kr; DUP050298112 ; roller* rom i IlL i :e of i usedl arger an ar cov, i 'll out in ease tbs f paint, mtil the esult m ng used? sfer an ill bei ivemen ie panel er-covli mediate jrepara- D5069 The American Society for Testing anti Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are Entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Yourcomments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a .fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.t Philadelphia, PA 1910$. DUP050298113 4 Designation: D 5087 - 91 Standard Test Method for Determining Amount of Volatile Organic Compound (VOC) Released from Solventborne Automotive Coatings and Available for Removal in a VOC Control Device (Abatement)1 This standard is issued under the fixed designation D 5087; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapprova!. A superscript epsilon () indicates an editorial change since the last revision or reapprovol. 1. Scope 1.1 This test method covers the determination of the amount of volatile organic compound (VOC) released from applied solventborne automotive coatings that is available for delivery to a VOC control device. This is accomplished by measuring the weight loss of a freshly coated test panel subjected to solvent evaporation or baking in a laboratory simulation of the production process. 1.2 This test method is applicable to the VOC released from flashoff and baking operations after the paint has been applied. 1.3 This test method is applicable to solventborne auto motive coating materials and is intended to represent or simulate the production process. The same general principles apply to waterborne coatings that contain volatile organic compounds (VOC), although specific procedural details are not presented herein to differentiate between VOC and water. 1.4 This standard does not purport to address the safety problems, if any, associated with its use. It is the responsi bility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: B 499 Test Method for Measurement of Coating Thick ness by the Magnetic Method: Nonmagnetic Coatings on Magnetic Basis Metals2 D1005 Test Methods for Measurement of Dry Film Thickness of Organic Coatings Using Micrometers3 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base3 D 1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base3 D2369 Test Method for Volatile Content of Coatings3 ' This test method is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcom mittee D01.23 on Chemical Analysis of Paints and Paint Materials, Current edition approved July 15, 1991. Published September 1991. Originally published as D 5087 - 90. Last previous edition D 5087 - 90. 2 Annual Book ofASTM Standards, Vol 02.05. -1 Annual Book ofASTM Standards, Vol 06.01. E 145 Specification for Gravity-Convection and Force J Ventilation Ovens4 2.2 EPA Standard: EPA Federal Reference Method 24--Determination o'ji Volatile Matter Content, Water Content, Density^ Volume Solids, and Weight Solids, of Surface Coatin 40 CFR, Part 60, Appendix A5 EPA-450/3-88-018, PB89152276--Protocol for Deti-mining the Daily Volatile Organic Compound Emissio Rate of Automobile and Light Duty Truck Topco Operations6 3. Summary of Test-Method 3.1 This test method simulates the loss of VOC from freshly coated surface by using the difference in weight of a coated test panel before and after baking. Metal test panels are subjected to a simulation of the production coating process including application, flashing, and baking. Th weight loss value obtained is then related to the volume solids deposited on the test panel to compute the number < pounds of VOC per gallon (grams per litre) of solids appliethat is available at the inlet of the VOC control device. 3.2 The information needed to determine the amount < VOC available for removal by the VOC control device is determined by identification of the points in the production! process at which coated objects would enter flashoff/bakin zones whose effluents are vented to the VOC control device,1 4. Significance and Use ~ 4.1 This test method provides basic engineering data thatj may be used to determine the amount of VOC available forn delivery at the inlet of a VOC control device (particularly fora the automobile industry).7 Typically, the procedure is useful f. for establishing the quantity of VOC that is evolved from the coating in the baking oven and available to be incinerated, although the same procedure can be followed for other forms; of VOC abatement (that is, carbon, adsorption, etc.), 4.2 This test method may be adaptable for use directly in a production environment if all the critical factors (for 4 Annual Book ofASTM Standards, Vol 14.02. 5 Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. 6 National Technical Information Services, 5285 Pori Royal Rd. Springfield. VA 22151. 7 United States Environmental Protection Agency Protocol for Determining the Daily Volatile Organic Compound Emission Rate of Automobile and Light Duty Truck Topcoat Operations, Ref EPA 450/3-88-018 dated December 1988. This protocol provides for VOC emissions reduction credit for abatement processes. 934 '''' W DUP050298114 # D 5087 expressed in pounds (grams) VOC per gallon (litre) solids applied: 11.1.1 The weight of coating solids deposited, Ws, is equal to the coated panel weight after full bake minus the panel weight before coating application as follows: Ws = W-i - W (3) or H-s = -- IV if W2 represents a fully cured paint film, where: Ws = weight of coating solids deposited, lb (g), W2 -- weight of panel at point which exhaust air is no longer vented to VOC control device, W3 = weight of panel with fully baked paint film, and W = weight of initial unpainted test panel. 11.1.2 Determine the weight of VOC available for abate ment control (WA) by taking the difference in the weight of the panel representing the point in the process at which the exhaust air is vented to the control device (IT,) and the weight of the panel at the point where the exhaust air is no longer vented to the VOC control device (W2) as follows: WA=Wt- W2 (4) where: WA = weight of VOC available for control, lb (g), W, = weight of panel at point at which exhaust air is first vented to VOC control device, and W2 - weight of panel at point at which exhaust air is longer vented to VOC control device. ;~ 11.1.3 Calculate the pounds VOC available for cohtrl per gallon of coating solids applied, CL, by combining tb weight of VOC available (WA), weight of coating soli, applied (Ws) and the coating solids density (Dcs) as folic v. <WA Dc (P where: CL = VOC loading Ib/gal (g/L), WA = VOC available for removal, lb, Ws = coating solids applied, lb, and 9> ( ! = coating solids density, Ib/gal (g/L). N"#' 2--Coating materials must be the specific formulations 1, as-applied condition) used in the process for which the VOC loadingf the VOC control device, is to be determined. 12. Precision and Bias 12.1 Precision--The precision of the procedure in thii method is being determined. 12.2 Bias--Since there is no accepted reference procedure I suitable for determining the bias for the procedure in this tesi>-' method, no statement on bias is being made. 13. Keywords 13.1 automotive coatings; solvent release; VOC abttc- i ment The American Society tor Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of:infringement of such-rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must to reviewed every five years and if notrevised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or foradditionalstandards and should be addressed to ASTM Headquarters. Your comments will receive carefut consideration at a meeting of the responsible technical committee, which you may attend. If you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Sfsndards, 1915 Race St., Philadelphia, PA 19103. 936 DUP050298116 st air is for contry' abining|| u>ng soli I as fol}0 M Designation: D 5095 - 91 Standard Test Method for Determination of the Nonvolatile Content in Silanes, Siloxanes and Silane-Siloxane Blends Used in Masonry Water Repellent Treatments*1 This standard is issued under the fixed designation D 5095; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision, A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. .Scope nutation C loadiii 1 This test method describes a procedure for the deter mination ofthe nonvolatile content (Ns) ofsilanes, siloxanes, ilblended silane-siloxane materials used in masonry water Client treatments and is applicable to both solvent- and Ster-bome materials. in this test1",j j1 2 This standard does not purport to address all of the ty problems, if any, associated with its use. It is the procedure ionsibility of the user ofthis standard to establish appro in this t J bate health and safety practices and determine the applica- fllty of regulatory limitations prior to use. For a specific rd statement, see Section 7. ' OC dbate-'V'ij 'I Referenced Documents "(1 ASTM Standards: H193 Specification for Reagent Water2 >3980 Practice for Interlaboratory Testing of Paint and "Related Materials3 145 Specification for Gravity-Convection and ForcedVentilation Ovens4 fgSummary of Test Method |.l A designated quantity of test material is weighed into preweighed aluminum dish containing the catalyst solugii, mixed, allowed to stand for 60 min at room tempera- and then heated in an oven at 110 SXT for 60 min. he nonvolatile content of the test material is calculated by btracting the solids of the catalyst solution from the total Bids by weight of the test solution. Significance and Use 14.1 This test method is used to determine the nonvolatile pntent of silanes, siloxanes, and silane-siloxane blended Materials used in masonry water-repellent treatments. It can used for the purpose of calculating the volatile organic bmpound (VOC) content of these materials under specified St conditions. [1 This test method is under the jurisdiction of ASTM Committee D-l on Faint l Related Coatings and Materials and is the direct responsibility of Subcom- H&ee DOt.47 on Masonry Treatments. [^Currentedition approved Sept. 15, 1991. Published November 1991, Originally iblished as D 5095 - 90. Last previous edition D 5095 - 90. Annual Book ofASTM Standards, Vols 6.03 and 11.01. I * Annual Book of ASTM Standards, Vol 06.01. 1A Annual Book ofASTM Standards, Vol 14.02, 5. Apparatus 5.1 Aluminum Dishes; 58-mm diameter by 18-mm high with a smooth (planar) bottom surface. Precondition the dishes for 30 min in an oven at 110 5C and store in a desiccator prior to use. 5.2 Forced Draft Oven, Type IIA or Type IIB as specified by Specification E 145. 5.3 Syringes, 1-mL and 5-mL. 5.4 Analytical Balance, capable of weighing to 0! 1 mg, 6. Reagents 6.1 Purity of Water--Unless otherwise indicated, refer ences to water shall be understood to mean reagent water as defined by Type IV of Specification D 1193. 6.2 p-Toluenesulfonic Acid, monohydrate.5 6.3 Alcohol, technical grade ethanol or isopropanol. 7. Hazards 7.1 In addition to other precautions, provide adequate ventilation, consistent with accepted laboratory practice, to limit the accumulation of solvent vapors. 8. Procedure 8.1 Catalyst Solution--Prepare a catalyst solution con taining a mixture of 0.5 % p-Toluenesulfonic acid in either ethanol or isopropanol. Thoroughly mix the solution. Pre pare sufficient catalyst solution to perform all tests. 8.1.1 The nonvolatile content of the test material can be calculated only if the same catalyst solution is used throughout the test,. Each time a new batch of catalyst solution is used, its nonvolatile content must be determined, 8.2 Determine the nonvolatile matter, in triplicate, of the catalyst solution as follows: 8.2.1 Weigh an aluminum dish to 0.1 mg. Record the weight as Wv 8.2.2 Using a 5-mL syringe, weigh 3 1.0 g, to 0.1 mg, by difference, of the catalyst solution into the preweighed aluminum dish. Record the weight of catalyst solution as Wy 8.2.3 Heat the aluminum dish containing the catalyst solution in a forced draft oven for 60 min at 110 5C. 8.2.4 Remove the dish from the oven and immediately place in a desiccator. Seal the desiccator and allow the dish to cool to ambient temperature. 5 Solutions of /J-Toluenesulfonic acid in isopropanol may be obtained from King Industries, Science Road, Norwalk, CT 06852. DUP050298117 ft D 5095 8.2.5 Reweigh the dish to 0.1 mg. Record the weight as W2. 8.2.6 Calculate the nonvolatile matter of the catalyst solution, iVC) in accordance with 9.1. 8.3 Determine the percent nonvolatile content, in tripli cate, of the test specimen as follows; 8.3.1 Thoroughly mix the test materials before use. 8.3.2 Weigh an aluminum dish to 0.1 mg. Record the weight as W4. 8.3.3 Using a 5-mL syringe, weigh 3 1.0 g, to 0.1 mg, by difference, of the catalyst solution into the preweighed aluminum dish. Record the weight as fV6. 8.3.4 Using a 1-mL syringe, weigh 1.0 0.1 g, to 0.1 mg, by difference, of the test specimen into the weighing'dish containing the catalyst solution. Record the weight ofthe test specimen as S, 8.3.4.1 Weighings must be done quickly to limit weight loss due to volatilization. If there is insufficient moisture present when testing solvent-borne silane materials, it is advisable to add up to 0.3 g ofreagent grade water to the dish containing the mixture of catalyst and test solutions. 8.3.5 Gently swirl the dish to mix the materials. Allow the materials to stand at room temperature for 60 min. 8.3.6 Heat the dish containing the mixture of catalyst and test solutions in a forced-draft oven.for 60 min at 110, 5C. 8.3.7 Remove the dish from the oven and immediately place in a desiccator. Seal the desiccator and allow the dish to cool to ambient temperature. 8.3.8 Reweigh the aluminum dish to 0.1 mg and record the weight as Ws. 8.3.9 Calculate the nonvolatile content, Ns, of the test specimen in accordance with 9.2. 9. Calculation 9.1 Calculate the nonvolatile matter, in the catalyst solution as follows: Nc = (W2- Wt)/W3 (1) where: N, nonvolatile matter of catalyst solution expressed as a decimal fraction, W, = weight of aluminum dish, g, W7 -- weight of dish plus catalyst solution after heating, g, and W3 = weight of catalyst solution before heating, g. 9.2 Calculate the nonvolatile content, Ns, in the test specimen as follows: N, = 100 - w4) - where: Ms = nonvolatile content of test specimen, percent, W4 = weight of the aluminum dish, g, Wi = weight of aluminum dish plus the catalyzed t material after heating, g, fV6 = weight of catalyst solution used in test specimen befi heating, g, ' iV= tion, (average of two determinations), and ' weight of test specimen before heating, g. 10. Report 10.1 Report the following information: 10.1.1 The average values obtained for the'nonvolatlp content of the catalyst solution, Nc. 'i 10.1.2 The average values obtained for the percent i volatile content of the test specimen, N%. , 11. Precision and Bias * 11.1 The precision estimated for this test method is basef on an interlaboratory study in which one operator in each five laboratories tested in triplicate on two different days lour- water repellent materials containing between 14 to 65 nonvolatiles. The results were analyzed statistically in ao.\n-' dance with Practice D 3980. The intralaboratory stan deviation was found to be 0,283 % absolute with 17 df ami,** the interlaboratory coefficient, of variation 7.02 % relmivey. with 16 df. Based on the standard deviation and coefficiai; . of variation, the following criteria should be used for judging*' at the 95 % confidence level, the acceptability of results. '1' 11.1.1 Repeatability--Two results, each the mean ofj riftll licates, obtained by the same operator should be considi icc'J,r suspect if they differ by more than 0.84 % absolute. * 11.1.2 Reproducibility--Two results, each the mean t triplicates, obtained by operators in different laboratories *- should .be considered suspect if they differ by more thaa|j 7.02 % relative. 11.2 Bias--Bias has not been established for this :.$G method. 12. Keywords 12.1 masonry water repellents; nonvolatile matter con tent; silanes; siloxanes The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, ore entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invitedeither forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to foe ASTM Committee on Standards, 7916 Race St., Philadelphia, PA 19103. $44 s l eri nwi .1 mr l.i 1/ forpf > sDOtl Current f Inmb Annual^ , Annual^.'; AnnuaM>' 1/ 938 DUP050298118 it Designation: D 5098 - 90 tliiSss 3W1 befofe Standard Specification for Artists' Acrylic Emulsion Paints*1 This standard is issued under the fixed designation D 5098; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon <} indicates an editorial change since the last revision or reapproval. lfia& blatill t 110,1- i baa iachof sloan 65 1 t acccri idani: t 'll anil elatLVo^ fficieal if ic Us. i>r til"sidereq ' an iJ atones s e than, i lis test. :r ccn- ijScope ;) This specification establishes requirements for compojn, physical properties, performance, and labeling of gts' acrylic emulsion paints. This specification covers pigments, vehicles, and addiRequirements are included for pigment identification, fastness, consistency, and drying time. Table 1 lists some pigments meeting the lightfastness iiremeats in this specification. In order to identify other bents that meet these requirements, instructions are for test specimen preparation. Test methods for aining relative lightfastness are referenced. The values stated in inch-pound units are to be jrded as standard. The SI units given in parentheses are Ihformation only. Referenced Documents h ASTM Standards: 1185 Test Methods for Coarse Particles in Pigments, | Pastes, and Paints1 ) 387 Test Method for Color and. Strength of Color Pigments with a Mechanical Muller2 )476 Specification for Titanium Dioxide Pigments2 1602 Specification for Barium Sulfate Pigments2 > 1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems3 1640 Test Methods for Drying, Curing, or Film Forma tion of Organic Coatings at Room Temperature3 > 3168 Practice for Qualitative Identification of Polymers in Emulsion Paints3 >4236 Practice for Labeling Art Materials for Chronic Health Hazards3 >4303 Test Methods for Lightfastness of Pigments Used in Artists' Paints3 > 4838 Test Method for Determining the Relative Tinting Strength of Chromatic Paints4 : 284 Terminology of Appearance5 Ifrerminology ' 5.1 Definitions: *5.1.1 colour index name--consists of the category (type of ye or pigment), general hue, and an assigned number given I This specification is under the jurisdiction of ASTM Committee D- L on. Paint L; Related Coatings and Materials and is the direct responsibility of SubcomjlStee DO 1.57 on Artist Paints and Related Materials. I Current edition approved July 27, 1990. Published November 1990. ^2 Annual Book ofASTM Standards, Vol 06.02. 1Annual Book ofASTM Standards, Voi 06.01. II Annual Bode ofASTM Standards, Vol 06.03. 1 Annual Bode ofASTM Standards, Vol 14.02. to a colorant in the Colour Index6 as an international identification system. 3.1.1.1 Discussion--For example, the Colour Index Name of one phthalocyanine blue pigment is Pigment Blue 15 (PB 15). 3.1.2 Colour Index Number--a five-digit number given in the Colour Index that describes the chemical constitution of a colorant. 3.1.2.1 Discussion--For example, the Colour Index Number of one phthalocyanine blue pigment is 74160. 3.1.3 Appearance terms used in this specification are defined in Terminology E 284. 3.2 Descriptions of Terms Specific to This Standard: 3.2.1 acrylic emulsion paint--paint containing a stable aqueous dispersipn of polymers or copolymers of acrylic acid, methacrylic acid, esters of these acids, or acrylonitrile; sometimes termed latex, acrylic latex, or polymer emulsion paint. 3.2.2 glycols--general term for dihydric alcohols used to provide freeze-thaw stability in acrylic and other water-based vehicle systems, 4. Significance and Use 4.1 This specification establishes quality requirements and provides a basis for common understanding among producers, distributors, and users. 4.2 It is not intended that all paints meeting the require ments be identical nor of uniform excellence in all respects. Variations in manufacture, not covered by this specification, may cause some artists to prefer one brand over another, either of which,may be acceptable under this specification. 5. Labeling Requirements 5.1 Pigment(s) Identification: ,5.1.1 Every label shall include for each pigment contained in the paint the information underlined in Table 1 which includes the Common Name, Colour Index Name, and any additional terms necessary to identify the form of the pigment. 5.1.2 The complete pigment identification given in Table 1, which also includes the Colour Index Number and a simple chemical description, shall be given in an appropriate producer publication. Manufacturers are encouraged to put this complete identification on the container label when label size permits. 5.1.3 The Common Name shall be placed on the front of the label and shall be the name of the paint except as 6 Colour Index, 3rd cd., 5 Vols and Revisions. The Society of Dyers and Colourists, London, 1971-75. Available from the American Association ofTextile Chemists and Colorists, P.O. Box 12215, Research Triangle Park, NC 27709. 939 DUP050298119 TABLE 1 Suitable Pigment List N%&' --Underlined information and the lightfastness rating in the table shall be included on every label. Key: Ughtfastness Category; Ughtfastness I Excellent Ughtfastness Ughtfastness it Very Good Ughtfastness Abbreviations used in Cofour Index Names: PB Pigment Blue PBk Pigment Black PBr Pigment Brown PG Pigment Green PO Pigment Orange PR Pigment Red PV Pigment Violet PW Pigment White PY Pigment Yeilow Pigment Notations: (CC) Concentrated sulfate. cadmium pigments may contain up to 15 % barium sulfate for color i control. Cadmium-barium pigments contain a much higher amount of barium^ W May darken in strong light (LF) Ughtfast type' <mns) Cotour index name or number not assigned Red shade (SM) Sensitive to moisture in direct sunlight (SS) . Sensitive to hydrogen sulfide .^ Colour Index Name Ughtfastness Category Acrylic Common Name and Chemical Class Colour Index Number ' * PY 109 -PY 1.10 PY 1,12 PY 13$ PY 139 PY 150 PY 151 PY 153 PY 154 PY 175 YELLOWS Aryflde YelloW G. with option of adding the name Hansa Yellow Medium, arytide yellow Aryiide Yeilow dOG, with option of adding the name Hansa Yellow Light, arylide yellow Cadmium Yellow. Light, concentrated cadmium zinc sulfide (CC) (SM) Cadmium-Barium Yellow Light, cadmium zinc sulfide coprecipitated with barium sulfate (SM) Cadmium Yellow Medium or Peep, concentrated cadmium sulfate (CC) (SM) CadmiUm-BariUm Yellow Medium or Deep, cadmium sulfide coprecipitated with barium sulfate (SM) Mars Yellow, .with option of adding the name Yellow Iron Oxide, synthetic hydrated- iron oxide Mars Orange, synthetic hydrated Iron oxide Yellow Ochre, natural hydrated iron oxide Nickel Tltanate Yellow, oxides of nickel, antimony and titanium Arylfde Yellow'RN, with option of adding Mansa Yellow RN, arylfde yellow Arylide Yellow GX, with.option of adding the name Hansa Yellow GX. aryfide yellow Arylide Yellow 5Gx, with option of adding Hansa Yellow 5GX, arylide yellow Diarylide Yellow HR7Q, dlarylfde yeliow Aryiide Yellow FGL, aryfide- yellow Arylide Yslloyv-IQQX, with option of adding the name Hansa Yellow 1QGX, arylide yellow Anthrapyrimldiiie Yellow, anthrapyrimidine Isoiridollnone; Yellow G,' tetVachtoroisoIndoiinane Isolndoiinone Yellow R/ telrachloroisoindolinone Flavanthrone Yellow, flavanthrone , Qulnophthalone Yellow, quinophthalone Isoihdoline Yellow, isoindollne Nickel Azo Yeitow, nickel complex azo Banzlmidazotone Yellow H4G. benzimidazolone Nickel Dioxins Yellow, dioxine yellow nickel complex .~ Benzimidazolone Yeilow H3G, benzimidazolone Benzimidazolone Yellow H6Q, benzimidazolone ORANGES Pinftrahinne Orange. dinitrahiline fSM) Cadmium Orange, concentrated cadmium suffo-selenide (CC) Cadmium-Barium Orange, cadmium suifoseienide coprecipitated with barium sulfate Cadmium Vermilion Orange, concentrated cadmium mercury sulfide (CC) Cadmium-Barium Vermilion Orange, cadmium mercury sulfide coprecipitated with barium sulfate Benzimidazolone Orange HL,' benzirrddazolons Perinone Orange, perinone Quinacridone Gold, quinacridone Quinacridone Deep Gold, quinacridone Benzimidazolone Orange HGL, benzimidazolone Benzimidazolone Orange H5G, manoacetolone REDS Naphthol ITR, naphthol ITR Naphthol AS-TR, naphthol AS-TR Naphthol AS-OL. naphthol AS-OL Naphthol AS-O, naphthol AS-0 11660 11710 77205 77205:1 77199 77199:1 77492 77492 77492 77789 . 11740 ` 11736 11741 21108 11767 11727 68420 NA 56280 70600 NA NA NA" 13980 NA 11761 11784 12490 12420 12460 12380 3 36 940 r ! DUP050298120 4! D 5098 Ughtfastness Category Acrylic TABLE 1 Continued Common Name and Chemical Class REDS (cont'd) Thioindigold Viofet, thioindigold Indian Red, synthetic red iron oxide (bluish hue) Light or English Red Oxide, synthetic red iron oxide (yelowish hue) Mars Red, with option of adding the name Red Iron Oxide, synthetic red iron oxide Mars Violet, with option of adding the name Violet Iron Oxide, synthetic iron oxide (violet hue) Venetian Red, synthetic iron oxide (yellowish hue) Light Red, calcined yellow ochre Vermilion, mercuric sulfide (OL) Cadmium Red Light. Medium, or Deep, concentrated cadmium-seleno sulfide (CC) - Cadmium-Barium Red Light, Medium, or Deep, cadmium seleno-sulfide copredpitated with barium sulfate I Naphthol AS-D. naphthol AS-D Cadmium Vermilion Red Light, Medium or Deep, concentrated cadmium mercury sulfide (CC) Cadmium-Barium Vermilion Rad Light, Medium or Deep, cadmium mercury sulfide coprecipitated with barium sulfate Naphthol Red, naphthol Quinacridone Magenta, y quinacridone Perylene Vermilion, perylene Perylene Red, perylene Bromlnated Anthranthrone, brominated anthranthrone Naphthol Red, naphthol carbamide H Naphthol Crimson, naphthol carbamide Benzimidazotone Maroon, bertzimidazolone Perylene Maroon, perylene , Thtoindicoid Magenta, thioinindigoid Naphthol AS, naphthol AS Perylene Red, perylene Quinacridone Red, y quinacridone red Pennone Red Deep, pennone Quinacridone Scarlet, quinacridone red Quinacridone Yellow Red, quinacridone red y Quinacridone Red, y quinacridone red PURPLES Ultramarine Red, complex Silicate of sodium and aluminum with sulfur Ultramarine Violet, complex silicate of sodium and aluminum with sulfur Quinacridone Violet, quinacridone violet b I Dloxazine Purple, carbazole dioxazlne Isovtolanthrone Violet isoviolanthrone BUIES Phthafocyanlne Blue, copper phthalocyanine Phthalocyanlne Blue, motet free phthalocyanine Indanthrone Blue, indanthrone Cobalt Blue, oxides of cobalt arid aluminum Ultramarine Blue, complex silicate of sodium and aluminum with sulfur Manganese Blue, barium manganate with barium sulfate Cerulean Blue, oxides of cobalt and tin Cerulean Blue, Chromium, oxides of cobalt and chromium Indanthrone Blue. Indanthrone ____ GREENS Phthalocyanine Green, chlorinated copper phthalocyanine Green Gold, with option of adding the name Nickel Azo Yellow, nickel chelated azo Chromium Oxide Green, anhydrous chromium sesquioxide Cobalt Green, oxides of cobalt and zinc Green Earth or Terra Verte. natural green Phthalocyanine Green, chlorinated and brominated phthalocyanine Light Green Oxide, oxides of nickel, cobalt, and titanium BROWNS Mars Brown, with option of adding the name Brown Iron Oxide, synthetic brown iron oxide or mixtures of synthetic iron oxides Burnt Sienna, calcined natural iron oxide Burnt Umber, calcined natural iron oxide containing manganese Raw Sienna, natural iron oxide Raw Umber, natural iron oxide containing manganese Colour Index Number 73312 77491 77491 77491 77015 77491 77492 77766 77202.1 77202:1 12370 77201 77201:1 NA 73915 71145 77137 56300 12475 12475 71513 71130 73360 12467 71140 NA 71100 NA 73902 73900 77007 77007 73900 51319 60010 74160 74100 69810 77346 77007 77112 7736B 77343 69600 74260 12775 77288 77335 77009 74265 77377 77499 77492 77492 77492 77492 941 DUP050298121 D 5098 Colour Index Name PBk 6 PBk 7 PBk 6 PBk 11 PW4 PW 6 . lightfastness. Lightfastness Category Acrylic i 1 l 1 1 l TABLE 1 Continued Common Name and Chemical Class Colour Index Number BLACKS Lamo Black, nearly Dure amorohous carbon Carbon Black, nearly pure amorohous carbon Ivory. Black, amorohous carbon Droduced bv charrina animal bones Mars Black, with option of addinq the name Black Iron Oxide, synthetic black Iron oxide WHITES Zinc White, zinc oxide Titanium White, titanium dioxide !rutile or anatase) with option of incfudina some barium sulfate or zinc oxide 77266 77266 77267 77499 77947 77891 thioindigoids have varying degrees c i ; described in 5.1.5 and 5.L6. Other identification may be placed elsewhere on the container. 5.1.4 The Colour Index Name may be spelled out in full or abbreviated depending on the size of the label. Example: Pigment Blue 15, or Pig. Blue 15 or PB 15. 5.1.5 Substituted Pigments--In the case of substituted pigments, the word "Hue" in equal size letters shall follow in the title, on the front ofthe tube, immediately after the name of the pigment that has been simulated. Directly below the title, the Common Name of the significant pigment used shall be given in letters no less than the next type size smaller than the title. For example: COBALT BLUE HUE {ULTRAMARINE BLUE). 5.1.6 Proprietary names or optional names may be used provided the Common Name(s) given in. Table ,1 appears on the front of the label directly under, the proprietary or optional name in letters no less than the next type size smaller than the proprietary or optional name. 5.1.7 Mixed Pigments--Artists' paints containing more than one colorant comply with this specification if all colored pigments used are on the suitable pigment list (Table 1) and provided the mixture itself has passed all other test requirements in this specification. The lightfastness category shall be that of the least lightfast pigment. This lightfastness category may be changed if these paints are tested for lightfastness in accordance with Test Methods D4303 and results indicating a different category are submitted to ASTM Subcommittee DO 1.57 for evaluation. 5.2 Provide on the label identification of polymer used in the paint N'(' )--The type of polymer can be identified by using Practice D 3168. 5.3 Lightfastness--The label shall contain the word "Lightfastness" followed by the appropriate rating, I or II, as ' given for each pigment in Table 1. 5.3.1 Lightfastness I pigments, when made into paint specimens as described in Section 7 and exposed, tested, and rated in accordance with Test Method D 4303, shall have a color difference (AE*ab) of 4 or less CIELAB units between the specimens measured before and after exposure. 5.3.2 Lightfastness II pigments, when made into paint specimens as described in Section 7 and exposed, tested, and rated in accordance with Test Methods D 4303, shall have a color difference (AE*ab) of more than 4.0 but not more than ' 8.0 CIELAB units between the specimens measured befo _ and after exposure. 5.3.3 Pigments were placed in a lightfastness category on the basis of either known historical performance in art works or the ratings irom four lightfastness tests conducted as described in Test Methods D 4303. Results from further tests on these, or other pigments, are solicited by ASTM Subcom mittee DO 1.57. 5.3.3.1 The lightfastness category of a pigment shall be changed if results from several further tests conducted ir accordance with Test Methods D4303 and approved by ASTM Subcommittee D01.57, establish a different lightfast ness category than the one given in Table 1. 5.3.3.2 Additional pigments shall be placed in Table 1 after they have been tested for lightfastness in accordance with Test Methods D 4303 and the test results submitted to ASTM Subcommittee D01.57 for evaluation, provided the results demonstrate that the pigments have the lightfastness ratings required for Lightfastness 1 or Lightfastness 11, as described in 5.3.1 and 5.3.2. 5.3.4 For information and to establish nomenclature, pigments in. Lightfastness III category are given in Table Xl.l in Appendix XI, but are not to be. used in paint conforming to this specification. These pigments have a color difference before and after exposure of more than 8,0 hut not more than 16.0 CIELAB units. 5.4 Toxicity--*A11 products and labeling must conform tb the Federal Hazardous -Substances Act and to Practice D 4236. 5.5 Statement of Conformance--"Conforms to ASTM Specification D 5098," or "Conforms to ASTM D 5098," or "Conforms to the quality requirements of ASTM D 5098," This statement may be combined with other conformance statements, such as, "Conforms to the quality and health requirements of ASTM Specification D 5098 and Practice D 4236." 5.6 Address--Include on the label (7) the name and address of the manufacturer or importer and (2) the country of manufacture. 6. Quality Assurance for Artists' Acrylic Emulsion Paints 6.1 Conditions not Covered in This Specification that Affect the Quality ofArtists' Acrylic Emulsion Paints: 6.1.1 Substrate--Factors such as the texture, gloss, effec tive pH, porosity, chemical composition, and condition of the substrate will affect gloss, gloss uniformity, drying time. jjUBjd: jHgpetifl 942 DUP050298122 D 5098 -__ cv. J h, i"** ton lK _ egreS^ljjl t| *3Slj or or} nu^ VOT^Sl/ ted jsnSj Li i , Lbcogjja nli Tw fed njJ1* Infast^ :.lblb 'Ijij u'aricfi " lied < eri tte'-. asuk^fl n':3 * latineil UK,'. psi la'C :ij'o an Ssfipj Mm i&t I.IJtKL _ ASIM* 5098.^ mancf, llLrtltf ractice' e and' )untm. iion, and the flexibility of the dried film. 1.2 Environmental Conditions--Factors such as temperpi humidity, air flow, and light conditions affect applica- properties. film formation, drying time, and adhesion. 1.3 Storage--Factors such as aging, and high and low |gi;atures may cause changes in consistency. Vehicles--Only acrylic polymer emulsions or acrylic jylymer emulsions may be used (see Note 1). Pigments--The pigments shall be limited- to those timmended for use in acrylic emulsion paints in the list of |f|ble pigments in Table 1. Their lightfastness rating shall |e numeral given in the same row. 4- Additives--Surfactants, preservatives, defoamers, gly| solvents, and thickeners may be used to achieve aging ifiity, to control foaming, to ensure freeze-thaw stability [film coalescence, and to obtain a desired consistency. | Inerts--Inerts shall -be included only to adjust product v s ot sheen, or to produce desirable working qualities. p 6 Preparation of Sample--Empty the contents of a vjously unopened container onto a glass slab and mix |oughly with a spatula to a homogeneous sample. "j Coarse Particles--Paints shall be free of oversize jeles. and shall form a uniform film. The maximum intent of coarse particles shall be 1 weight % as determined Test Methods D 185. 8 Fineness of Dispersion--Determine the fineness of persion by Test Method D 1210. For paste paint: on a plate, using a spatula, mix the paint with an equal ume of water until homogeneous. The maximum allowjje grind reading is 1.5 mils (40 pm). ? Consistency--Paints shall be smooth and creamy. The ste type of paint shall not flow or level when applied with alette knife. [10 Freeze-Thaw Stability--Using a freezer that has a pcraturc of 20F (--7C) or lower, subject the paint to five gv.e-thaw cycles.- A freeze-thaw cycle shall consist of `Zing the paint to a solid state (minimum of 18 h) and n thawing the paint to room temperature (minimum of 5 The paint shall then meet the requirements of 6.7, 6.8, d 6.9. Jft 11 Drying--Use a 6-mil (150-p.m) clearance film applifoi to make a uniform drawdown on a lacquer-sealed nt (. At a relative humidity of 50 to 75 % and a tempera te of 65 to 80F (18 to 27C), the dust-free drying time, tci mined in accordance with Test Method D 1640, shall be t toss than 10 min. 12 Tinting strength requirements will be included in this cification as appropriate tinting strength standards for ividual pigments are established. Test Method D 387 may used to determine the tinting strength of pigments or its when all ingredients are known. Test Method D 4838- be used to determine the relative tinting strength of matic paints containing a single pigment and the same |icle but where other ingredients are unknown. mill i '/ .i edt-cion of' time, |Lightfastness Determination J7.I If a pigment is not listed in Table 1, test specimens of paint containing the pigment shall be prepared. These test gcimens shall be tested in conformance with the require- nts for exposure and evaluation given in Test Methods 4303. N)*' 2--A report of the results of these tests may be submitted to ASTM Subcommittee DO 1.57 for inclusion of the pigments in Table 1 The report shall include information on lest conditions, instruments used, and be accompanied by the test specimens, which will be returned. 7.2 Materials: 7.2.1 Aluminum Exposure Panels,7 3 by 6 in. (75 by 150 mm). 7.2.2 Posterboard, lightweight, approximately 20 mils (0.5 mm) thick, having a glossy finish on one side. 7.2.3 Titanium Dioxide Acrylic Emulsion Paint. 7.2.4 Spray Apparatus, for applying ground coats. 7.2.5, Paint Brush, 2.5 in. (60 mm) wide for applying ground coats if spray apparatus is not available. 7.2.6 Soft Hair Brush, 1 in. (25 mm) wide for applying ground coats to aluminum panels. An oxhair artist's "stroke" brush is suitable. 7.3 Specimen Preparation: 7.3.1 Ground Coats: 7.3.1.! For the first ground coat under acrylic emulsion paints, prepare the following enamel: Weight % Medium oil length soya alkyd, 50 % nonvolatile Rutile titanium dioxide9 (conforming to Type II of Specification D 476) Blanc fixe (conforming to Specification D 602) Driers: 0.15% zinc and 0.15 % zirconium as - metal on the alkyd nonvolatile Sufficient mineral spirits for milling 1 ' 20 40 40 7.3.1.2 Mill to a Hegman fineness of 7 as measured by Test Method D 1210. Thin with mineral spirits to appro priate vistdsity for spraying or for flow coating by brush. 7:3.2 For the second ground coat for acrylic emulsion paints, prepare the following enamei: Weight % Medium oil length soya alkyd, 50 % nonvolatile8 Rutile titanium dioxide9 (conforming to Type II of Specification D 476) Colloidal silica10 Driers: 0:15 % zinc and 0.15 % zirconium as metal on the alkyd nonvolatile Sufficient mineral spirits for milling 40 30 ' 30 7.3.2.1 The colloidal silica may be dispersed separately in mineral spirits using a high-speed mixer and added to the milled alkyd-titanium pigment paste. Mill to a Hegman fineness of 7 as measured by Test Method D 1210. Use sufficient mineral spirit for proper application. N)*' 3--These soya alkyd enamels are used for the ground coats because of their color stability, nonabsorbency, adhesion of the spec imen coats under humid conditions, and freedom from blistering that can occur with an acrylic ground coat under high humidity. 1 The No. A-36 aluminum panel manufactured by Q Panel Co., 26200 First St., Cleveland, OH 44145. has been found satisfactory for this purpose. " The following alkyd resins have been found satisfactory for this purpose: Cargill, No. 5196; 1MC McWhorter, DURAMAC 2419: Reiclihold. No. 11-035; and Spencer-Kellog, AROPLAZ 1082 M5G. 9DuPonl R900 rulile titanium dioxide, available from E.l. du Pont de Nemours & Co., 1007 Market St., Wilmington. DF. 19898. has been found satisfactory for this purpose. 10 Syloid 308, available from Davison Chemical, Div. W,R. Grace Co.; PC Box 2117; Baltimore. MD 21203. has been found satisfactory for this purpose. 943. DUP050298123 7.3.3 Application ofGround Coats: 7.3.3.1 Degrease aluminum substrates before applying the ground coat. 7.3.3.2 Apply one coat of the enamel described in 7.3.1.1, followed by one coat of the enamel described in 7.3.2. To flow coat the aluminum panels for sun exposure use a 1-in. (25-mm) soft hair brush. Coat the postetboard to be used for laboratory exposure on the less absorbent, glossy side. N+,' 4--Coating the posterboard is most conveniently done on the whole sheet before cutting to size. 7.3.3.3 Allow a minimum of five days drying time fol lowing the first coat and two weeks or more after applying the second coat and before applying the paint to be tested. 7.4 Mixing Whites for Dilution ofColors: 7.4.1 Use a white containing the same emulsion and additives as the formulation in which the pigment is incor porated if possible.11 The following basic composition has been found satisfactory: Weight % Acrylic emulsion nonvolatile Rutile titanium dioxide9 (conforming to Type II of Specification D 476) 23 to 24 34.6 7.4.1.1 Keep the viscosity ofthe mixing white to 250 P or slightly lower. 7.5 Preparation ofTest Paints: 7.5.1 The pigment to be tested may be milled in a compatible paste for acrylic emulsion. If a prepared artists' paint of known composition is available, it may be used for this test instead of.preparing a dispersion. 7.5.2 Dilute the pigment paste or paint with the white containing the same type of vehicle until the spectrophoto- metric measurement of the dried film shows 35 to 45 % relative reflectance at the wavelength of maximum absorp tion for that pigment. The wavelength of maximum absorp tion is located at the point of lowest reflectance on the spectral curve between 420 and 620 nm. If using a tristimulus filter colorimeter, the lowest of the three filter readings is the region of maximum absorption and the dilution should be adjusted so that a reading of 35 to 45 % reflectance is obtained with this filter. The diffuse white reference standard for all measurements should have an absolute reflectance between 97 and 100 %. 7.5.2.1 To obtain this reflectance, use the Kubelka-Munk 11 If the acrylic vehicle composition of the paint is Unknown, Rhoplex AC-234, from Rohm & Haas Co., Independence Mall W., Philadelphia, PA 19105, is compatible with most acrylic emulsion paints. Single Constant Method described in Appendix X2 or uses trial and error method. 7.5.3 Make instrumental readings with the specular refltc, tance included to minimize the effect on readings of anv' change in gloss and to minimize the effect of brush strain 7.5.4 Use an applicator with a 6-mil (150-pm) aperture to make a minimum size drawdown, 1 'A by IV2 in. (40 by -i mm), or other minimum size appropriate for the viewin' area of the instrument used. Return all recoverable paini tu the batch to allow for repeat mixes and measurements. 7.5.5 For acrylic emulsion paints, 80 g of white paint is|j|j needed since paint used in the drawdown is lost. `* 7.5.6 For the initial weights of white stated in 7.5.4 :)n,_ j 7.5.5, the weighing must be accurate to 0.05 g. 7.6 Application ofPaints to Panels: ! 7.6.1 Prepare four specimen panels on appropriate sufi.'# strates for each pigment under test. Two are used in the first ` lightfastness tests and two are retained in subdued light, one Jfor visual comparisons with the exposed panels and one in 1 case a third test ismeeded to supplement results from the first two tests, as described in Test Methods D 4303. 7.6.2 Apply the test paints by brush to the alurainuffii'sd panel if exposure is to be under glass to the sun or by brusftJS to the posterboard panel if exposure is to be to laboratory i apparatus. _1 7.6.3 Using the No. 12 artist's flat bristle brush, brush the "1 panels lengthwise, then crosswise, and again lengthwise, ttus^J time with a light touch to produce a film as smooth aPp possible. The mixing whites must be fluid enough m facilitate leveling, but not have excess vehicle that can aii'cct* j# the test. Do not use thinners. Apply two coats to all specimen lUi panels to achieve complete opacity. "If* , an 7.6.4 Allow specimens to dry between coats as described Wm tr in the Procedure section (Dry-Through or Dry-to-Handla^ Hckne Time) of Test Methods D 1640. After recoating, allow par specimens to dry hard, as described in the Procedure section Jgfnceo (Dry-Hard Time) of Test Methods D 1640, before measuring '< them prior to exposure. Acrylic paints can be recoated the >' J^cfiocta next day and read two days after recoating. Hote;N;. 8. Exposure me - 8.1 Conduct exposure tests, calculate mean color differ ence, and assign pigments'to lightfastness categories as described in Test Methods D 4303. acre: 9. Keywords 9.1 artists' acrylic paints; lightfastness; quality require ments; test specimens 944 DUP050298124 : Oi>! # D 5098 APPENDIXES (Nonmandatory Information) XI. LIGHTFASTNESS III ft The pigments in Table Xl.l are not sufficiently jst to be used in paints that conform to this specifica` These pigments are listed here solely to establish common terminology. They may be satisfactory when used full strength (without dilution) or with extra protection from exposure to light. ^ir Index iparne Iri7 iri46 23BS Ms Lightfastness Category AcryJic Ilf HI 111 M TABLE XI.1 Lightfastness 111 Common Name and Chemical Class Naphthol Red AS-D, naohthol Naphtha! Red. naohthoic arvlida Dioxazine Purple, carbazole dioxazine Hooker's Green, ferric-nflroso-beta-naohthol Colour Index n Number 12390 12485 51319 10006 X2. KUBELKA-MUNK SINGLE CONSTANT METHOD FOR PREPARING PAINT FILMS 40 5 % REFLECTANCE HnnuhV V bnKbjj ioiatStv: 1.1 Prepare a mixture of white and colorant in propor|estimated to give a paint having a reflectance of 30 to | at the wavelength of maximum absorption. Calculate rusjirtlfi '.- th'is J Concentration of colorant in white in this batch as "Vs: oofi* ce= Wc/Ww+ wc rngll :n a*rifr Kg: = concentration of colorant, and Bnd Wc -- weight of white and colorant, respectively, v' lil! seme Handled all8$ SCLlitjf lasunn itea the f $ used in the batch. |gv or brush a film of this paint over contrast paper at a fitness sufficient to give complete visual hiding. |g. 1.1 After allowing the film to dry, measure the reflec- ; of this film at the wavelength of maximum absorption a spectrophotometer or, if using a colorimeter, the stance with the filter that gives the lowest reading (see X2.1). Calculate the Kubelka-Munk Single Constant ue of this reflectance as follows: differiries isC: equtre-1 (K/S)m = [1 - (Rm - 0.04)]3/2(Rm - 0.04) = Kubelka-Munk Value, = reflectance measurement of the mixture, made with the specular component included ex pressed as a decimal value, and = decimal value correction for surface reflectance. X2. [--To speed drying, accelerated methods may be used. It is |mmended that water-based acrylic paints be warmed to 50 to 55"C t h after 1 b of air drying before measuring tire reflectance. Placing drawdowns of oil paints near fluorescent lamps, for example in the I? jfescent light exposure racks described in Annex A1 of Test Methods 003, will speed their drying time. 2.1.2 Calculate the Kubelka-Munk absorption coeffiSit for unit concentration as follows: Kc - (K/S)JCc |re Kc = unit absorption coefficient. 2.2 Based on the results of the trial mixture, calculate I concentration of colorant in white required to give the desired 35 to 45 % reflectance at the wavelength of max imum absorption as follows: Cd = (/f/5W^c = 0.4500/^. where Cd -- concentration of colorant in white predicted to give a paint with the desired 35 to 45 % reflectance value. X2.3 Adjust the concentration of the trial batch so that the concentration of colorant equals Cd. Determine the changes in colorant concentration, AC as follows: AC = Cd -- C0 These changes are positive ifthe trial batch has a reflectance greater than 40 % and negative if the reflectance is less than 40 %. If AC is positive, add more colorant to the trial batch to bring the concentration of colorant to Cd. If AC is negative, add more white to bring the concentration of colorant to Cd. Because it may be necessary to add large amounts of white to correct for concentrations of colorant giving reflectance values far below 40 %, it is usually best, to prepare a trial batch expected to give a AC value..that is moderately positive or only slightly negative. X2.3.1 For the case where AC is positive, the weight of colorant needed to prepare a second batch is, AWC=*WC- Ca(Ww + KQ/Q - I x (L.F.) where: AWC = weight of colorant to be added to the trial batch to obtain a corrected batch with a colorant concentra tion of Cd, and L.F. = "loss factor" = weight of paint from trial batch used to prepare the corrected batch/weight of paint prepared as trial batch. The loss factor, L.F., allows for paint removed to prepare drawdowns, loss by transfer to different containers, etc. This term may be neglected if losses are small compared to the batch size. The other terms are as defined in the previous sections of this appendix. X2.3.2 For the case where AC is negative, the weight of white needed to prepare a corrected batch corresponds to, AW,, = WC- + Wc)/Cd X (L.F.) 945 mmmtmL DUP050298125 D 5098 where A W,, = weight of white needed to adjust the colorant concentration in the batch to Cd. Other terms are as defined above or in previous sections of this appendix. X2.4 Prepare a paint film from the adjusted batch. After drying, measure the reflectance at the wavelength of max imum absorption. If this value does not fall within 35 t(* 45 %, repeat X2.3 through X2.4, where C, now becomes ftfe Cc for the next batch correction. Normally only a iteration is necessary and a second batch correction will no * be needed. .jits The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such pa et nt rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee andmust be reviewed every five years and if not revised, either reapproved or withdrawn. Yourcomments are invited either for revision of thisstandard or for aetctitional.standards and should be addressed to ASTM Headquarters. Your comments wilf receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have not received a fair hearing you should mafce your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. jff v ' 946 .. .... DUP050298126 fb Designation: D 5107 - 90 Standard Practice for Preparatory Surface Cleaning of Architectural Sandstone1 This standard is issued under the fixed designation D 5107; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the'year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. pcope 11 This practice covers non-abrasive surface cleaning of kitectural sandstone to remove grease, dirt, loose mate; and surface deposits such as soot, fly ash, hydrocarbon piues, and algae and other biological growth in preparafor the application of water repellent coatings. Procefes include broom cleaning, vacuum cleaning, air blast fining, water cleaning (and detergent water cleaning), and finical cleaning. f.2 Limitations--This practice is intended to dean archiitural sandstone without damaging it or altering the surface profile. '1.3' This standard does not purport to address all of the tyfafety problems associated with its use. It is the responsibility jBthe user ofthis standard to establish appropriate safety and tfiulth practices and determine the applicability ofregulatory Imitations prior to use. For specific hazard statements, see Action 4. ^Referenced Documents -|l ASTM Standards: j$C 119 Definitions of Terms Relating to Natural Building Stones2 |? 4262 Test Method for pH of Chemically Cleaned or Etched Concrete Surfaces3 j)P4263 Test Method for Indicating Moisture in Concrete '' by the Plastic Sheet Method3 p 4285 Method for Indicating Oil or Water in Compressed Air3 it. Significance and Use 1^, 3.1 Surface cleaning is necessary to prepare architectural indstone surfaces for application of coatings intended for ater repellent protection. Surface cleaning of the sandstone bstrate helps to ensure proper adhesion of the coating. (3.2 Use of procedures described in this practice may not ! adequate where protective systems will be used for ontinuous or intermittent immersion' or mechanical lading. Hazards J4.1 Moisture in the architectural sandstone may be detri mental to coating adhesion or (in some cases) cure. Moisture r|ntent shall be in compliance with coating manufacturer's 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee Mj)l.47 on Masonry Treatments. I| 1 K^AC. urrent edition approved Nov. 21, 1990. Published January 1991. Annual Book ofASTM Standards* Vol 04.08. P Annual Book ofASTM Standards, Vol 06.01. recommendation. See also Test Method D 4263. 4.2 Localized staining (for example efflorescence and metallic staining) and previously applied coatings or preserv ative treatments not compatible with the treatment may require removal by other surface preparation methods. 4.3 Water cleaning, detergent water cleaning, and chem ical cleaning should notbe performed at temperatures below 40F. 4.4 Many chemical cleaning products contain acids and should be handled according to manufacturers' recommen dations. Use and" disposal of materials should conform to established federal, state, local, and project requirements. 4.5 If pressure washing equipment is employed for water cleaning or for flushing the surface With detergent water cleaning or chemical cleaning, the minimum effective pres sure should be used. Avoid excessive pressures that could damage the sandstone substrate. 5. Procedure 5.1 Air blast, water, scrubbing, sweeping, or vacuuming are acceptable cleaning methods. Chemical cleaning agents may be used to Temove surface deposits such as soot, fly ash, and hydrocarbon residues not removed by any of the above methods. Chemical cleaning should be preceded arid fol lowed by a thorough fresh water rinse. 5.2 Existing conditions of the substrate will determine the selection of appropriate procedure(s). Prior to the initiation of cleaning, small test areas should be cleaned in inconspic uous areas by the selected procedure to determine effective ness. 5.3 The six types of cleaning procedures are described below. One or more of the procedures may be required to remove contaminants from-the sandstone surface: 5.3.1 Broom Cleaning--Removes most loosely adherent solid contaminants. 5.3.1.1 Working from top to bottom, sweep the surface with a clean industrial stiff-bristled broom or similar device. Remove sweepings from the immediate work area. 5.3.1.2 Clean broom-cleaned surfaces again using one or more of the surface preparation procedures specified in 5.3.2 through 5.3.6. 5.3.2 Vacuum Cleaning--Removes surface dust and other debris. 5.3.2.1 Vacuum the surface with a heavy-duty type indus trial vacuum to provide an essentially dust-free surface. 5.3.3 Air Blast Cleaning--Removes debris, dust, dirt, loosely adherent architectural sandstone, and laitance from walls to provide an essentially sound, dust-free surface. 5.3.3.1 Clean surface with a compressed-air stream through a blasting nozzle held at an oblique angle approxi mately 2 ft (0.6 m) from the surface. Air stream pressure 947 h i- I I' fe'. DUP050298127 D 5107 should not exceed 100 psi (689 kPa). 5.3.3.2 Before initiating air-blast cleaning, verify that the air stream is free of oil in accordance with Test Method D4285. 5.3.3.3 Surface cleanliness is dependent upon carrying off airborne dust before it is redeposited. Vacuum cleaning may be required to remove redeposited dust. 5.3.4 Water Cleaning--Removes dust, dirt, and water- soluble surface contaminants. 5.3.4.1 Clean the surface with a stream of clean potable water, aimed at an oblique angle approximately ^ ft (0.6 m) from the surface, having sufficient pressure to remove dust, dirt, and loose material without damaging the substrate. When necessary, hand scrub with a nonmetallic stiff-bristled fiber brush. 5.3.4.2 Prior to water cleaning, make provisions for the removal of wash water and contaminants generated. 5.3.4.3 If necessary, test the cleaned surface for moisture content in accordance with Test Method D 4263 prior to applying coatings. 5.3.5 Detergent Water Cleaning--Removes water-soluble surface contaminants and oils, grease, and other emulsifiable materials on the surface. . 5.3.5.1 Scrape off heavy deposits of grease or oil and prewet the surface with potable-water. Clean the surface with a nonmetallic stiff-bristled fiber brush, using an aqueous solution of detergent or nonsolvent emulsifier. Immediately after treatment, before the surface dries, remove residues of the cleaning agent by thoroughly flushing the surface with clean potable water. Repeat flushing until the pH of the surface water meets the acceptance criteria of Test Method D 4262, 5.3.5.2 Repeat 5.3,5.1 until water does not bead on the surfaces. ', 5.3.5.3 Prior to detergent water washing, make provisions for the removal of wash water and cpntaminants generated. 5.3.5.4 If necessary, test the cleaned surface for moisture content in accordance with Test Method D 4263. 5.3.6 Chemical Cleaning--This procedure is similar to detergent water washing, but involves the use of proprietary chemical cleaning compounds (generally hydrofluoric and phosphoric acids) lor the removal'ofsurface deposits such as soot, fly ash, and hydrocarbon residues. N-.' --In some cases, removal of heavy soiling may require use alkaline pretreatment prior to acidic cleaning. ! 5.3.6.1 Chemical cleaning using acidic products is gen r- ally not recommended for calcareous sandstones. (See De ~ nitionsC 119.) 5.3.6.2 Protect all adjacent materials and surrouni areas as recommended by the manufacturer of the proi etary chemical cleaning compound. . 5.3.6.3 Prior to chemical gleaning, provide for applieati. to small test area to determine effectiveness. Make provisi mj for the removal of water and contaminants generated during full-scale cleaning operations. 5.3.6.4 Before applying the chemical cleaning compouBofi prewet the surface thoroughly with potable water to pn vent. ` absorption of the cleaning solution within the pores of .he 1 masonry. V- 5.3.6.5 Apply a dilute solution of a proprietary cleaning'll i <1 compound to tlje pre-wet surface as recommended by thesSl (' C " manufacturer. Leave the cleaning solution on the surface fo^Jj Ep' a prescribed dwell period (usually less than 5 min). jfaj,, 5.3.6.6 Immediately following the dwell period, and be~& fore the surface dries, flush thoroughly to wash chemical mir; cleaning compounds from the surface, then nnse thoroiK-hly-d; rfn.t / from bottom to top. (Rinsing from bottom to top helps n> avoid surface streaking.) Repeat flushing may be necessary to; remove cleaning residues. 5.3.6.7 Evaluation--Visually examine the prepared n- mm* face to evaluate removal of debris, dust, dirt, oil, gmas^gm^fi \ loosely adherent sandstone building stone, and other con taminants. Test the surfaces cleaned with proprietary chem^S leal cleaning'compounds for pH in accordance with Tes Method D 4262 and if necessary test for moisture content /< ^ accordance with Test Method D4263 prior to applying coatings. 5.4 Surface cleaning is intended to provide a clean, contamination-free surface without damaging or removing architectural sandstone from intact, sound surfaces. Accept able surfaces shall be free of oil, grease, loosely adher.rt !.' sandstone, and other contamination such as dirt, soot,' f ash, and hydrocarbon residues. The American Society for Testing and Materials takes no position respecting the validity of anypatent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressfy advised that determination of the validity ot any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. . This standard is subject to revision atony time by the responsible technical committee and must Pa reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either tor revision of this standard or for additional standards end should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair bearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. kelateE nb.Doifi; Birrcntfe UnnuaW 948 fi DUP0502981 28 Ijv) Designation: D 5108 - 90 i require u.w Ij lets is gener:s. (See Dei, ' J'js Standard Test Method for Organotin Release Rates of Antifouling Coating Systems in Sea Water1 surrounding f the prop f This standard is issued under the fixed designation D 5108; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A r application superscript epsilon {<) indicates an editorial change since the last revision or reapprovat. ce provisions rated dunng Scope J This test method covers the laboratory determination compound 1$^ rate at wll'ch organotin expressed as tributyltin (TBT) :r to pie veqi Igrieased from an antifouling (AF) coating in synthetic sea pores of thajMflr us`nS graphite furnace atomic absorption spectroBtometry (GF-AAS). This does not exclude the use of hary cleaning ana*ytical methodology for measurement of organotin nded by :ht .- ' CJ water such as gas chromatography, e surface "toi i4?l - The values stated in SI units are to be regarded as in). Jjfijdiird. The inch-pound units given in parentheses are for iod, and b; li>froation only. soluble tin (tributyl- and triphenyltin) that occur during a period of immersion under specified conditions of constant temperature, pH, salinity, and low heavy-metal concentra tions in the surrounding sea water. Quantitative measure ment of the release rate is necessary to help in selection of materials, in providing quality assurance, and in under standing the performance mechanism. 4.2 This test method serves only as a guide for organotin release rates in service. Organotin release rates of antifouling (AF) paint systems in service can vary over the life , of the coating system depending on the formulation and the sh chemical- JHP standard does not purport to address all of the i thoroughly 3wlktvproblems associated with its use. It is the responsibility top helps to jjjpie user of this standard to establish appropriate safety necessaivto mSy-tiees and to determine the applicability of regulatory stations prior to use. For specific hazard statements, see repared sur-,1 Son 7. oil, grease;.i,, I other con-^i Referenced Documents etary chcme with Tcse contenL in to applying H ASTM Standards: gl141 Specification for Substitute Ocean Water2 11212 Methods for Measurement of Wet Film Thickness Hof Organic Coatings3 Je a clean Dr removim 1114138 Test Method for Measurement of Dry Film (Thickness of Protective Coatings by Destructive Means3 environment. Differences in berthing locations, operating schedules, length of service, condition of paint-film surface, temperature, pH, and salinity can affect results. Results obtained may not necessarily reflect actual tributyltin release rates that will occur in service, but provide reliable compar isons ofthe release rate characteristics of different antifouling formulations. 4.3 This test method will serve to characterize the early, release rate pattern, as well as estimate the steady state release, oftributyltin from both self-polishing copolymer and free-association antifouling paints. 5. Apparatus 5.1 Release-Rate Measuring Container--A 2-L (nominal 'h gal) polycarbonate container,4 approximately 13.5 cm (5.5 ces. Acc^p `,ly adhering, irt, soot, fl luminary of Test Method || The candidate paint system is applied to cylindrical Ipecimens. The coated specimens are placed in a tank of Retie sea water where the tin levels are kept low by plating the sea water through a carbon filter. At specified ,|vals, each specimen is placed in 1500 mL of unused sea JjSr and is rotated for 1 h. The rate of tributyltin release Spin the paint is determined by measuring tributyltin centrations in the sea water. ;2 Analysis of sea water for tributyltin is conducted by Jtiacdng the organotin with toluene, washing with sodium Siroxide, and measuring for total tin using (GF-AAS). in.) in diameter and 19 cm (7.5 in.) high, fitted with three polycarbonate rods approximately 6 mm (nominal 'A in.) in diameter to serve as baffles. Rods shall be evenly spaced on the inside circumference of the container to prevent swirling ofwater with the test cylinder during rotation. The rods will be secured to the container walls using acetone or methylene chloride. 5.2 Constant Temperature Bath--A temperature con trolled water bath capable of maintaining a temperature of 25 2C into which one or more release rate measuring test containers can be placed.5 5.3 Holding Tank--A container of such dimensions so as to permit immersion of four or more test cylinders; must be ^Significance and Use equipped with a system to continuously circulate synthetic sea water in the tank through a carbon filter. The rate of Si This test method is designed to provide a laboratory water flow and the size Of the carbon filter should be selected jgfpedure to measure changes in the release rates of solvent to maintain tributyltin concentrations below 100 pg/L. Flaw his test method is under the jurisdiction of ASTM Committee D-l on Paint .elated Coatings and Materials and is the direct responsibility of SubcomD01.45 on Marine Coatings. irreivt edition approved Dec. 5, 1990. Published February 1991. Xntmal Book ofASTM Standards, Vol 11.02. ' mtiaf Book ofASTM Standards, Vol 06.01. 4 A Nalgene Container, available from Cole-Palmer, 7425 N. Oak Avc., Chicago, IL 60648, catalog number R-6761-20, or equivalent, has been found satisfactory for this purpose. ' 5 Boekel Water Baths, Models 148003 and 148004 available from Boekel Industries Inc., 509-T Vine St., Philadelphia, PA 19106, or equivalent, have been found satisfactory for this purpose. 949 DUP050298129 # D 5108 rates should generally be set to obtain 2 to 8 turnovers per h. The size and geometry of the tanks as well as the positioning of the inflow and outflow ports for the water circulation system should be selected to obtain a slow, relatively uniform flow of synthetic sea water past all test cylinders in the tank. Maintain the pH of the synthetic sea water between 7.8 and 8.2, and the salinity between 30 and 35 parts per thousand (ppt). The tank shall be provided with heaters to maintain the temperature between 21 and 27C (70 and 81F). 5.4 Test Cylinders--Approximately 6.4 cm (nominal 2xh in.) outside diameter polycarbonate pipe coated with a 10-cm band of AF paint around the exterior circumference of the test cylinder to provide 200 cm2 of paint film that can be immersed and freely rotated in the release rate measuring container. Seal the bottom Of the test cylinder with a polycarbonate disc using acetone, methylene chloride, or a polycarbonate cement so as to form a watertight joint. Do not coat the bottom 1 to 2 cm of the test cylinder. The test cylinder shall be of such height so that a rotating device can be attaphed to rotate the cylinder and the upper open end of the cylinder is above the level of the test container immer sion liquid to prevent entry of the immersion liquid into the test cylinder. 5.5 Test Cylinder Rotating Device--The device shall be capable of rotating the test cylinder in the release rate measuring container at 60 5 f/min. No part of the device shall be immersed in sea water.6 5.6 Centrifuge Tubes, 50-mL capacity, with screw closures7 (or disposable bottles, culture tubes, separatory funnels, etc.) made of polycarbonate, TFE flourocarbon, or borosilicate glass. 5.7 Mechanical Shaker, with appropriate holders. 5.8 Dispensers, automatic or repeating, for reagents. 5.9 Pipets, with disposable polypropylene tips. 5.10 Graphite Furnace, atomic absorption spectropho tometer (GF-AAS) with automatic sampler. 5.11 pH Meter, with a mercury/mercurous chloride (Hg/ Hg2Cl2) electrode. 5.12 Appropriate Volumetric Flasks. 6. Reagents and Materials 6.1 Synthetic Sea Water--Substitute ocean water in ac cordance with Section 6 of Specification D1141 or a proprietary equivalent with a salinity of 30 to 35 ppt. 6.2 Extraction Solvent--Toluene, spectrograde or equiva lent. 6.3 Tributyltin Standards--Prepare standards using a stock solution of tributyltin chloride (reagent grade, min imum 96 % pure) in methanol (suggested concentration of approximately 10 mg/L). The standards are acidified with acetic acid (less than pH 4) to obtain a stable solution. 6.4 Hydrochloric Acid (HC1) (10 % aqueous solution). 6.5 Hydrochloric Acid (HC1) (0.IA). 6.6 Nitric Acid (HN03) (10 % aqueous solution) can be used in place of HC1 to clean labware. 6 A six-paddle stirrer, Model 300. manufactured by Whitaker Medical Mfg. Co., Phipps and Bird Div., 8741 Landmark Rd., Richmond, VA 23228, or equivalent, has been found satisfactory for this purpose. 7 Oak Ridge Tubes, available from Cole-Parmer, or equivalent, have been found satisfactory for this purpose. 6.7 Sodium Hydroxide (NaOH) (3 % aqueous solution! t be tre 6.8 Sodium Hydroxide (NaOH) (0.1 A'). m HC1 <i 6.9 All reagents and cleaning agents used must be tin jijpugbly ' Iso be 7. Hazards Prepa 7.1 Warning--Antifouling paints contain toxic mated that could cause skin and eye irritation on contact adverse physiological effects if ingested or inhaled. jn3 preparation of test specimens and the application of variJ types ofpaints, the use of appropriate protective clothing a| equipment is required consistent with local, state, and fede' government regulations, and recognized industrial and tei nical standards. Spills, overspray, and unused mate! should not be flushed down the drain, but should be dispose of as hazardous waste. iag 7.2 See antifouling paint supplier's Material Safety 1 Sheet. in t re tube Prep ite 14 siori of itnain \ Jjior cir( 3 Pain! I prior ^ beyond " typical jntainei 1.4 Appf 8. Calibration and Standardization srior cirj 8.1 Prepare three standards throughout the range of til quantification limit to 100 pg of tin per litre by dilution j toluene of a stock solution oftributyltin chloride (96 % pu in methanol. Include one standard with a concentration d approximately 50 pg of tin per litre. An alternate range < concentrations may be used when appropriate. 8.2 Prepare synthetic sea water spiked with three coriO_ trations of TBT in the range of 10 to 50 pg of tin per litre ! spiking with stock solution of tributyltin chloride in ih|| anol. When the concentration of tin extracted iri'toluefl exceeds 100 pg/L appropriate dilution should be emplo to keep it within the limits ofthe calibration curve (0 to if flg/L). 8.3 Operate the graphite furnace in accordance manufacturer's instructions. Optional conditions are dej scribed in Appendix X1. 8.4 Analyze the following: 8.4.1 At the beginning of each instrument run, perforl analysis of the toluene blank and standards in toluene |jj d of/! rinirnujit, lufactii:.' At a if rs horn) piy as rri', trkeied 4 applic* |C. I '.5 Estiti ldestruo' king tej conclui ' nnent <t. Test M(' |ke sever estini . .cknesS s . For IQ order to establish that the response of the instrumental be great. linear. Plot separate calibration curves for each analysftfflj .in 50 pi. the standards (peak height absorbance versus tin CQncentjjl 9.6 Plaf tion), and calculate the slope, intercept, and coefficient qfj 'ter the determination for each curve using least squares regressip|l j|ore sets k> or another appropriate procedure. Id one cep 8.4.2 Sea Water Blank--Extract and analyze as specified (e cylind|!-- for test samples to establish baseline. stationi, 8.4.3 Spiked Sea Water Samples--Extract and analyzes (rough specified for test samples to determine extraction efficiency.-S , 9.7 M4 Recovery must be 90 to 110%. lectrode)v 8.4.4 If changing the graphite tube during a run ifg holdii'; necessary, the blank and standards in toluene should bef |ther 0.1|; analyzed to ensure proper response and linearity beforej 'ays and ftJ continuing the sample analysis. eekly.\f : 8.5 Determine the tin concentration of individual test j fore th| samples with reference to the 50 gg/L calibrating standard juent i * analyzed immediately after those test samples. some mditior 9. Procedure 9.8 Afi 9.1 Organotins have a strong tendency to adsorb on | certain glass or plastic surfaces. Therefore, ali labware. (glass or polycarbonate) used for organotin release measurements lays, tra|? leasuringv. Sea wateif 950 DUP050298130 # D 5108 *9, |be treated as follows: .clean thoroughly by soaking in fHCI or HNOj for a minimum of 6 h. Rinse labware ' ghly with distilled water and allow to dry. Cleaning Iso be accomplished by soaking in concentrated HQ. for fPrepare all samples, blanks,' and standards' in labware fte ntaclll ft 3f VI,'J, i in this manner. Disposable materials (pipet tips, cen.`tubes, etc.) do hot have to be acid-washed before use. . Prepare tile exposure surfaces (200 cm4) of three fate test cylinders to provide a suitable surface for p;oh ofthe paint system to ffe applied. Mask the surfaces adfe nn'te(^ mu di` liain uncoated (including the bottom 1 to 2 cm of the )>r circumferential surface of the test cylinder). Paints shall be manufactured a minimum of seven Iprior to testing. Also, test paints shall not be allowed to ieyond the manufacturer's recommended shelf life. Pro *at> T > typical storage conditions during aging, that is, sealed in ptainer commonly used for sale and held at 20 to 30C. Apply one or more coats of antifouling paint to the jior circumferential surface of a test cylinder to produce ge'cjf ilutiqH ) % ml 'aiuiV, rand |nciof AF paint with an exposure surface of 20Qcm2 and limum dry film thickness of 100 pm (4 mils),.Follow iufacturer's instructions with respect to mixing and dryAt a minimum, mechanically shake until the paint ap- homogeneous. Apply using a sponge applicator or |y as recommended by the manufacturer. If the paint'is uen&t* rketed only in spray cans, then apply as a spray. After the ' lurih 11 ' niif I toll mpkm, lOtiM application allow the paint to dry for 7 1 days a*;23 to ie. ];5 Estimate the initial dry film thickness using a suitable idestructive method such as Method D 1212. If the |hing tests exceed 6 months measure the filmi thickness at conclusion of the test. Methodology for the final mea- lie \\r ! JIO ;ment can be either that used for the initial measurement Test Method D 4138. If a .nonstandard method is used, te several film thickness measurements for. each cylinder estimate the variability of the determination. Film perornw luene; cness should remain greater than 50 pm; throughout the For tests of long duration, the initial thickness may need uti^rr ji, Cbe greater than 100 pm to maintain a thickness greater alrbsiolj m 50 pm throughout the test. acentjjggj |9.6 Place all cylinders in a single batch in a holding 'tank icien^gS :r .the 7-day drying period. A batch consists of one. or igressipgj >re sets of three replicate cylinders coated with a test paint specifi|jj| id one control (unpainted) cylinder. The painted surface on cylinders must be completely submerged. Cylinders must stationary and positioned so that sea water moving ial\/- >> |rough the tank will flow around each cylinder. ficiencj' : 9.7 Monitor the pH (using a pH meter with a calomel Jectrode) and the temperature of the synthetic sea water in run is- le holding tank daily. Adjust the pH if necessary using ould be* be Fore| ler 0.! Ar NaOH orO.l/VHCl. Quantitate salinity every 14 tys and adjust if necessary. Determine TBT concentrations ual test tandard' feekly. When TBT levels increase, change the carbon filter rfore the TBT concentration exceeds 100 pg/L. More requent monitoring of synthetic sea water may be -necessary some instances to maintain the specified environmental mditions. 9.8 After 1, 3, 7, 10, 14, 21, 24, 28, 31, 35, 38, 42, and 45 orb ays, transfer all cylinders in given batch into individual -e (glass ( teasuring containers containing 1500 mL of fresh synthetic -ements j ba water. Randomly assign cylinders (control and painted) to measuring containers at each leaching. When transferring cylinders, lift the cylinder out of the holding tank, allow sea water to drain off, install the cylinder into the rotating device, and submerge the painted area into the sea water. Immediately start rotation of the cylinder at 60 5 r/min, and continue rotation for 60 min. When transferring the cylinders, do not touch or in any way damage the paint Fdm, and dp not allow the paint surface to dry. The transfer should be completed as quickly as possible (generally, in less than 5 min). 9.9 If testing beyond the minimum (45 days) length requirement is desired, the study may he extended to 73 days.,,During the. extended test, remove the cylinders from the holding tank every 3 to 4 days to make a me,asurement of the leach-rate. 9.10 At the completion of the cylinder rotation, immedi ately remoye the cylinder from the measuring tank and return it to the holding tank. Pipet. a 25-mL subsample ofthe sea water into.a 50-mL centrifuge tube containing sufficient 10% HCi to reduce the pH to <4.0. If the number of samples from the leach measuring steps exceeds the daily analysis capacity, the samples may be refrigerated and stored in the acidified state.in a sealed container for up to 14 days. Clean the measuring containers using appropriate proce dures (distilled water or acid wash) before reuse. 9.11 Partition acidified sea water samples with 10 mL of toluene (1.5 min shaking on a mechanical shaker). Remove most of the toluene and wash it with 5 mL of a 3 % aqueous NaOH solution (10 min shaking). Pipet off (or separate using a separatory funnel) the organic phase and analyze for total tin content by GF-AAS. The toluene extract can be stored sealed in the dark at 4?C for up to 24 h before analysis. 10. Calculation 10.1 Calculate the concentration ofthe TBT cation in the sea water of the measuring container as follows: CTBT = (C X- E x F)/S where: CTBT = concentration of TBT cation (pg/L), C = concentration of tin in the toluene extraction Oig/L), E = volume of toluene -- 10 mL, F = correction factor to convert tin to TBT = 2.5, and S' = aliquot of sea water analyzed = 25 mL. This equation can be simplified as follows if the prescribed volume of sea water and toluene are used: tVoT = (Csn x 30 x 2.5)j25 = O'sn 10.2 Calculate the release rate by the following formula: R = (C0' 0 x-Vx D)/(Tx A) where: R = release rate (gg/cm2/day), D = 24 h/day, K = 1.5L, volume of sea water in measuring container, T = 1 h during which cylinder is in measuring container, and A = 200 cm2 surface area of paint film. This formula can be simplified as follows: DUP050298131 D 5108 R = (CTBT x 1.5 x 24)/(l X 200) " ^*1' 1 x 0.18 10.3 Calculate the 14-day cumulative release of TBT cation as follows: R = R, + (2 x R3) + (4 x R7) + (3 x Rl0) + (4 x i?I4) where: R -- 14-day cumulative release, [xg/cm2 14 days, and /J,, J?3, R-!, Ri0, and i?i4 = release rates for sampling days 1, 3, 7, 10, and 14, respectively, jig/cm2 per day. 10.4 Calculate the average release rate (pg/cm2 per day) by averaging individual release rate measurements taken from day 21 through the last day of sampling (day 45 through day 73). If values at day 21 are high and it is suspected that the release had not reached pseudo steadystate conditions, then compare the release rate at day 21 to the mean for all release rates from day 21 through the termination of testing (45 to 73 days). If the release rate exceeds the mean by two or more standard deviations, then the release rate may be excluded from the average. If the day 21 release rate is excluded, the day 24 release rate may be evaluated by the same procedure. 11. Report .11.1 Report the following information: 11.1.1 Report the concentration in micrograms per.L, ofTBT cation in the sea water of the measuring tank and,t rate of TBT cation release (micrograms per square cei metre per day) for each sampling time (give values individual replicates as well as the mead). Plot the rate ! TBT release as a function of time (use linear axes), , report the 14-day cumulative release and the average rel< rate. 12. Precision and Bias 12.1 Precision and bias for this test method have not l determined. 13. Keywords 13.1 antifouling-coating system; organotin; release TBT; tributyl tin APPENDIX (Nonmandatory Information) XI. GRAPHITE FURNACE OPERATING INSTRUCTIONS XI. 1 Operate the graphite furnace in accordance with the guidelines that have been used by two operators. manufacturer's instructions. Tables XI. 1 and XI.2 provide TABLE X1.1 Navy Equipment--for Toluene Extraction N23' --Light Source: Tin electrodeless discharge lamp (EDL) Wavelength: 224.6 nm . Background Corrector. On Step Temperature, "C Ramp Time, s Hold Time, s Gas Flow (mL/mln) 1. Dry 2. DryA 3. Char 4. Atomize .. 5. Clean 6. Cool 100 110 1000 2000 2700 20 5 5 10 0 2 2 10 300 5 300 2 300 8 0 5 600 15 300 A 286.3 nm tin hollow cathode. B Gas stop stage must be used after Step 2 to prevent the carrier gas sweeping organotin out of the tube. c Stop gas. TABLE X1.2 Perkin-Etmer 4000AS fitted With A Perkin-Elmer 500 Graphite Furnace With Temperature Programmer N45' --Light Source: Hallow cathode lamp Wavelength; 266.3 nm - Step 1. Chart* 2. Ash 3. Atomize 4. Clean Temperature, C 250 900 2600 2700 Ramp Time, s Hold Tima, b ' Purge gas used: argon. XI. AUTOSAMPLER X2.1 Perkin-Elmer AS40Aulosamplers--This autosampler has been used with the Perkin-Elmer HGA 500 graphite a Available from Perkin-Elmer Corp., 761-T Main Ave., Norwalk, CT 068590001, or equivalent, has been found suitable for this purpose. furnace. The autosampler introduces aliquots of 20 (xL into the graphite tube. Each sample is analyzed three times and an average given. The machine automatically recalibrates after every 12 samples. llMlIlliii iii 952 DUP050298132 D 5108 DUP0502981 33 # D 5108 X4. DESCRIPTION OF PROPOSED TESTING APPARATUS X4.1 A 200 cm2 organotin antifouling paint film of a minimum 100 pm thickness is applied to the curved surface of a polycarbonate cylinder closed at one end. This cylinder is suspended with its closed and immersed within and concentric with a larger polycarbonate cylinder holding synthetic sea water. The coated internal cylinder is rotabout its axis at 60 5 r/min in order to p peripheral speed of about 1 knot. In practice, the comn 3 dally available polycarbonate "multipurpose jars" descr! in this test method will hold 1500 mL of synthetic sea wn isl N67' 1 --Test Container Dimensions: Capacity, L 2 Inside diameter, cm 12.7 Outside diameter, cm 13.3 Height {without cover), cm 19 N89' 2--Rotating Test Cylinder Dimensions: D = approximately 7 cm (2Va in. nominal), H *= 12 cm min, L ~ 10'Cm coated section, and X = 1 -cm uncoated band. FIG. X4.1 Dimensions of Testing Apparatus (Container and Cylinder) The American Society for resting and Materials takes no position respecting1 the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and Ifnot revised, either reapprovad or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race $t., Philadelphia, PA 79703. 954 D4<;; D-C, . n--}, u'l. 'Cun f- DUP050298134 Designation: D 5139 - 90 Standard Specification for Sample Preparation for Qualification Testing of Coatings to be Used in Nuclear Power Plants1 This standard is issued under the fixed designation D5139: the number immediately following the designation indicates the year of original adoption or, in the ease of revision, the year oflast revision. A number in parentheses indicates the year oflast reapprovaJ. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. "cope |1 This specification defines the size composition and ice preparation requirements for test samples used to Pate coatings according to the following ASTM test "dures. eferenced Documents ASTM Standards: ,36 Specification for Structural Steel2 ' 33 Specification for Concrete Aggregates3 : 150 Specification for Portland Cement4 192 Practice for Making and Curing Concrete Test Specimens in the Laboratory3 260 Specification for Air-Entraining Admixtures for Concrete3 494 Specification for Chemical Admixtures for Concrete3 1618 Specification for Fly Ash and Raw or Calcined Natural Pozzolan for Use as a Mineral Admixture in Portland Cement Concrete3 >3911 Test Method for Evaluating Coatings Used in Light-Water Nuclear Power Plants at Simulated Design Basis Accident (DBA) Conditions5 >3912 Test Method for Chemical Resistance of Coatings Used in Light-Water Nuclear Power Plants3 D4060 Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser5 ip4082 Test Method for Effects of Radiation on Coatings Used in Light-Water Nuclear Power Plants5 'D4256 Test Method for Determination of the Decontaminability of Coatings Used in Light-Water Nuclear Power Plants5 .`D 4258 Practice for Surface Cleaning Concrete for Coat ing5 D4259 Practice for Abrading Concrete5 D4260 Practice for Acid Etching Concrete5 D4541 Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers5 1 This specification is under the jurisdiction of ASTM Committee D-33 on tectivc Coating and Lining Work for Power Generation Faculties and is the irect responsibility of Subcommittee D33.02 on Service and Material Parameters. Current edition approved Dec. 12, 1990, Published January 1991. 3 Annual Book ofASTM Standards, Vol 01.04. 3 Annual Book ofASTM Siandards. Vol 04.02. 4 Annual Book ofASTM Standards, Vo! 04.01. * Annual Book ofASTM Stundardss Vol 06,01. 2.2 Other Siandards: American Concrete Institute, ACI 301 Specifications for Structural Concrete for Buildings6 SSPC-SP-1, 2, 3, 5, 6, 7, 10, or ll7 3. Significance and Use 3.1 This specification provides uniform requirements for the preparation of test samples used for qualification testing of coatings used in nuclear power plant construction and maintenance. 4. Steel Samples 4.1 Sample size shall be a minimum of 2 in. wide by 4 in. long by Vs in. thick. Edges and corners may be rounded. A 'M in. diameter hole suitably located may be in the test panel as appropriate for the test samples in Test Methods D39I1, D 3912,0 4082 and D 4256. 4.1.1 For Test Method D 4541 the minimum size shall be 3 in. wide by 5 in. long by Vi in. thick. 4.2 All panels should be carbon steel, meeting the require ments of Specification A 36. 4.3 Surface preparation shall be in accordance with SSPCSP 10 for qualification testing. Other surface preparation as required by the project or specific conditions may be used when testing for evaluation over surfaces other than SSPCSP 10, such as SSPC-SP 1, 2, 3, 5, 6, 7, or 11. 5. Concrete Blocks 5.1 Applicable to Test Methods D 3911, D 3912, D4082, D4256 and D4541. The minimum size shall be 2 in: by 2 in. deep by 4 in. long. The edges may be chamfered up to 'U in. maximum. ___ 5.2 Composition shall be as follows: Cement Gravel Sand Air-entraining ad mixture Water-reducing admixture Pozzolan Water, demineral ized or distilled Specification C 150, Type II Specification C 33, size Vs in. Specification C 33 Specification C 260 Specification C 494 Specification C618 7 sacks/yd3 45 % by volume 55 % by volume As recommended 4 to 7 % As recommended As recommended to 15 % amount 3 in. slump 6 Available from American Concrete Institute. P.O. Box 19150. Detroit, MI 48219. 7 Surface Preparation Standards are available from Steel Structures Painting Council, 4400 5th Ave., Pittsburg. PA 15213-2683. ! 955 DUP050298135 Nominal 1 Cubic Foot Batch Cement Gravel Sand Air-entraining ad mixture Pozzolan Water-reducing admixture (Type A) Water, demineral ized or distilled Specification C ) 50, Type f! low alkali Specification C 33, Size Vs in. Specification C 33 Specification C 260 22.2 lb 45.3 lb 55.5 lb 31 mL Specification C 618 Specification C 494 2.2 lb As recommended by the manufac turer As required to pro duce 3-in. slump (approximately) 5.3 Blocks shall be cast horizontally in forms using release . agents that are compatible with the coatings to be used. The top surface, as cast, shall be given a broom finish, unless otherwise specified. The block surface is to be covered with plastic during the first 24 h to simulate water curing unless a curing compound is included in the testing. 5.4 The block shall be removed from the form after 24 h and wet cured in accordance with ACI301 or Practice C 192. 5.5 If a curing compound is to be used, apply the compound to the broom finished surface immediately after finishing and to all other surfaces of the block within 2 h after its removal from the form. 5.6 Allow the block to cure for 28 days in accordance with ACI 301 before application of the coating system unless otherwise specified. 5.7 After curing, remove loose material on the broom finish .surface by light wirebrushing. Remove loose material on the cast surfaces by blowing with air (80 to 100 psi) unless otherwise specified, such as Practices D 4258, D 4259, or D 4260. 5.8 All surfaces of the blocks shall be coated in accordance with Test Method D 3912. The upper and/or lower ends of the blocks shall be left uncoated for all other testing. 5.9 A suitable hanger compatible with the testing appa ratus shall be affixed at the mid-point ofthe upper end of the block where applicable. 5.10 Large bug-holes, rock pockets and other coating defects may be simulated by drilling holes to test coating systems for patching surface defects. 6. Miscellaneous Materials 6.1 Follow 4.1 and 4.3 for metallic materials such as aluminum, galvanized steel, and other metals. 6.2Follow 5.1 and 5.3 for castable materials such grout, fireproofing, and other castables. 7. Abrasion Test Samples 7.1 Substrate material for abrasion testing shall be of i size in accordance with Test Method D 4060 and shall |' aluminum or steel and of a thickness to maintain a surface after surface preparation. "; 7.2 Surface preparation shall be compatible with coating to be tested. ' 8. Application 8.1 All test samples shall be coated with the full coati system including any applicable fillers. The manufactur 'jj latest published application instructions shall be followed t ij mixing and coating application unless otherwise speci ij Any special procedures or conditions shall be noted in the \ documentation including thinning, mixing, drying/cunng;j times, force curing, aging between coats/systems, interne-j diate surface preparations or other special procedure*, nr j conditions. 8.2 The film thickness range shall be representative cl t ( j specified work for which the testing is being conducted. 8.3 Test samples for maintenance painting test program* j may include simulated aging ofthe existing coating, interme^ 1 diate surface preparation and wide ranges of coating film5'! thicknesses. Field conditions should be duplicated as close as i is possible including coating application methods that may j differ from the manufacturer's published data. 9. Documentation 9.1 The procedures and conditions used for the -tes?* sample preparation shall be documented. As a minimum 1 documentation shall include preparation times and dates, j surface preparation details, coating sequence and individual | dry film thickness ranges of each coat, total thickness range, j environmental conditions, and product batch identification.; 9.2 Record all deviations from the procedures called for in. this Specification, that is, all items allowing "unless otherwise: specified" that are different than those described, g 10. Keywords i 10.1 concrete blocks; nuclear power plants; qualification i testing; sample preparation; steel samples; test samples gi The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users o1 this standard are expressly advised that determination of the validity of any such patent rights, and the risk oi infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must fee reviewed every five years and if notrevised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to A$TM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards. 1916 Race St., Philadelphia, PA 19103. 1S.1coTpehJi| coat dear pfi * this guidg ing and fy Pmsibilhy ff prrent ed| 956 DUP050298136 Designation: D 5144 - 91 :> ( I< , 1 he slia'i in . 1 coatiiil Standard Guide for Use of Protective Coating Standards in Nuclear Power Plants1 Tliis standard is issued under the fixed designation D 5144; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year pf last revision. A number in parentheses indicates the year ofiastreapprovai. A superscript epsilon (e) indicates an editorial change since the last revision or reapprovai. INTRODUCTION 1 coattail actuu-, t.j owjlfiic 1 specific :d in thS ig/cunnf inK-rnc. du: o- hijiS ve of the ? ted. *roj'iam< intcmie^ in| film ; closea hat Tiaj jj the usj' num thft'i d ditc>., diviauri ft is range, fication ed for id therwise I ificatiou les Protective coatings (paints) have been used extensively in the nuclear industry to protect the surfaces of facilities and equipment from corrosion and contamination by radioactive nuclides in'' accordance with ALARA. In the absence of a standard method of selecting, testing, and evaluating coatings, many sites evaluated paints by empirical tests to determine which were useful in their particular operation. Understandably, the methods of testing were not uniform throughout the industry. It has been very difficult, consequently, to compare the results obtained at one site with those obtained at another. Standard tests whereby industrial (nuclear) users ofpaints systematically prepare specimens and subject them to selected evaluations, thus permitting uniform comparisons, are advantageous, internationally as well as domestically. The designer of light water-moderated nuclear reactor systems must consider the possibility of a Design Basis Accident (DBA) and the subsequent events which might lead to the release or expulsion of a fraction of the fission-product inventory of the core to the reactor containment facility. Engineered safety features, principally a reactor containment facility, are provided to prevent the release of fission products to the biological environment during and after this improbable event. The design, fabrication, quality assurance, and testing of these engineered' safety features ensure reliable operation and safety under all anticipated conditions. Large areas of the reactor-containment facility are painted with a protective coating. If severe delamination, peeling, or flaking causes significant portions ofthe coating to be discharged into the common water reservoir (primary containment sump), the performance ofthe safety systems could be seriously compromised by the plugging of strainers, flow lines, pumps, spray nozzles, and core coolant channels. The safety requirement for protective coatings is to ensure that failure of the coatings under DBA conditions does not adversely affect the performance of post-accident fluid systems. Therefore, coatings must be qualified to the environmental exposures anticipated during normal plant operation, and during DBA and other upset conditions. This guide is the result of a comprehensive examination of the experience and data that have been developed on protective coatings in the nuclear industry over approximately 40 years. Standards pertaining to nuclear coatings have historically been covered by ANSI N5.12, N101.2, and N101.4. Responsibility for updating, rewriting, and issuing appropriate ANSI replacement standards has been transferred to ASTM, 'specifically ASTM Committee D-33, on Protective Coating and Lining Work for Power Generation Facilities. Quality assurance in the nuclear industry is a mandatory requirement for all aspects of safety related nuclear coatings work. The objective of this guide is to provide a common basis on which to define and specify the performance requirements for the coatings which will be used in Service Level I and II areas of a nuclear facility. Proposed Regulation 10CFR50.65 (Draft Rule November 28, 1988) defines the requirements for an effective program for maintenance of nuclear power plants. This guide may be used both for coatings applied to new nuclear power plants and to facilitate implementation of the coating aspects of 10CFR50.65. Scope mi 1.1 This guide provides a common basis on which protecjftive coatings for the surfaces of light water-moderated "Tfoclear power generating facilities may be qualified and g1 This guide is under the jurisdiction of ASTM Committee D-33 on Protective g)ating and Lining Work for Power Generation Facilities and is the direct ssponsibility ofSubcommittee D33.02 on Service and Material Parameters. jf&Ctirrent edition approved Jan. 8, 1991. Published March 1991. selected by reproducible evaluation tests. This standard also provides guidance for application and maintenance of pro tective coatings. Under the environmental operating and accident conditions of nuclear power generation facilities, encompassing Pressurized Water Reactors (PWR's) and Boiling Water Reactors (BWR's), coating performance may be affected by exposure to any one, all, or a combination of the foEowing conditions: ionizing radiation; contamination by radioactive nuclides and subsequent decontamination DUP050298137 D 5144 processes; chemical and water sprays; high-temperature highpressure steam; and abrasion or wear. 1.2 The content of this guide includes: Section ' Referenced Documents Terminology 2 3 Significance and Use 4` Preparation of Test Specimens Radiation Resistance Decontamination Physical Properties Chemical Resistance Fire Evaluation DBA Testing ' .. . : ! - 5' 6 7 8. 9 10 11 ' Surface Preparation, Coating Application; and:lnspection.for, 12 Shop and Field Work .. - Quality Assurance 13 Keywords \, 14 1.2.1 In addition, this -guide'addresses technical topics within ANSI N5.12 and ANSI N101.2 that were covered by separate ASTM standards, for example, surface preparation, shop and field and coating application, and shop and field. 1.2.2 Applicable sections of this guide and specific accep tance criteria may be incorporated into specifications and other documents where appropriate.2 1.3 This standard'does Hot purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents.- 2.1 ASTM Standards: ' D3843 Practice for Quality Assurance for Protective Coatings Applied to Nuclear Facilities3 D3911 Test 'Method fdr Evaluating Coatings used in Light-Water Nuclear Power Plants at Simulated Design Basis Accident (DBA) .Conditions3 D3912 Test Method for Chemical Resistance of Coatings Used in Light-Water Nuclear Power Plants3 D4060 Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser3 D4082 Test Method for Effects of Radiation on Coatings Used in Light-Water Nuclear Power Plants3 D4227 Practice for Qualification'of Journeyman Painters for Application of Coatings to Concrete Surfaces! Of Safety-Related Areas in Nuclear Facilities3 ' D4228 Practice for Qualification of Journeyman Painters for Application of Coatings to Steel Surfaced of Safety- Related Areas in Nuclear facilities3 D4256 Test Method for Determination of the Decontaminability of Coatings Used in Light-Water' Nuclear Power Plants3 ' < D 4537 Guide for Establishing Procedures to Qualify and Certify Inspection Personnel for-Coating. Work in Nu clear Facilities3 D4538 Definitions of Coating and Lining Facilities3 Terms Work Relating to for Power Pri, Gone ertiSj - 3 D4541 Method for Pull-Off Strength of Coatings L Portable Adhesion Testers3 D 5139 Specification for Sample Preparation for Qualms tion Testing of Coatings to be Used in Nuclear pJSL Plants3 er E 84 Test Method for Surface Burning Characteristics ,;i Building Materials4 2.2 Other Standards: 'IB ANSI N5.12 Protective Coatings (Paints) for the Nucii*.,"-' , Industry5 1-11 ANSI N101.2 Protective Coatings (Paints) for Light WaSH Nuclear. Reactor Containment Facilities5 11 ., ANSI N1QL4 .Quality Assurance for Protective Cc,.ii . -,:1 Applied to Nuclear Facilities5 10CFR50.65. Draft rule "Ensuring the Effectiveness n> * . . Maintenance Programsfor Nuclear Reactor PLi November 28, .19886 Lg , Regulation Guide L54 Quality Assurance Requirements*, for Protective Coatings Applied to Water-CooleJ clear. Power Plants6 i.jj USNRC Review Plan 6.1.2 Protective Coating Sysieiri^j (Paints). Organic Materials6 __ . 10CFR20.1(C). Standards for Protection Against Reua- ' tion; Purpose6 U$NRC Regulation Guide 8.8 Information Relevant in li Ensuring that Occupational Radiation Exposuies At\' Nuclear Power Stations Will Be As Low As Is Reasnnif , ably Achievable.6 ih.. 3. Terminology . 3.1 Definitions--'Dchmilons for use with this guide a?fl shown in Definitions D 4538 or other applicable stanc u 3,2 Descriptions of Terms Specific to This Standard 3.2.1 ALARA---the concept of reducing radiation esgo ' Si,H sure-to personnel to levels "as low as is reasonably achiev-jjj|?'-Rij . able " as defined in the USNRC Regulation Guide 8.8, and* 10CFR.20.KC). 3.2.2 Coating Service Level I--areas where-coating failure could adversely affect the operation of post-accideni fluid systems and, thereby,. impair safe shutdown. Witli -w exceptions, Coating Service Level I applies to coatings inside primary containment 3.2.3 Coating Senice Level II--areas where c.- iti _ failure could impair, but not prevent, normal operating performance. The function of Coating Service Le . H My. <U4 t?'-i T coatings is to provide corrosion protection and i jjfeihoc]. decontaminability in those areas outside primary contain fr. 9.2 ment subject to radiation exposure and radionuclide con laractfi- tamination. ted i^<; fd aWJf. 4. Significance and Use |. Fill' 4.1 This guide addresses the concerns of Regulation Guide 1.54 and Standard Review Plan 6.1.2, and the 2 Certain ASTM standards are available in compilation form (which includes this guide), as Compilation of ASfhi Standards for Use of Protective Coating Standards in Nuclear Power Pfdnts For expedicnt reference and usage by personnel involved in nuclear coating work. ;: ! - 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vol 04.07. 5 Available From American National Standards Institute, 11 W. 42nd St., 13lf* Floor, New York, NY 10036. 6 Available from the U.S. Government Printing Office, Washington, DC 20402. . pneraf I *ot ex| facility! 958 D U P O50298138 05144 %< 'pp jjgement of ANSI Standards N5.12,N101.2, and N10! .4. aide covers coating work on previously coated surfaces I as bare substrates. The entire document applies to all |g work in Service Level I areas. Applicable sections of aide may be used to evaluate and select protective pgs for Service Level II areas. ctya' |H[ - i'oiy ^IjjJ feparation of Test Specimens i! All test samples used for qualification testing of jigs shall be prepared in accordance with Specification `9. ' I!C*i1PpI Idiation Tolerance Tests it ( Coating film resistance to radiation exposure shall be Ihted in accordance with Test Method D 4082. 11 ,.'*or ;i^T fijjSL itemsail scontamination Test The relative decontaminability of the coating shall be Rated by Test Method D 4256. |l Certain coatings may contaminate more readily than |ts, and the responses to decontamination treatments also . In some cases, the desired level of decontamination |be achieved merely by cleaning the coating surface; in cases, decontamination may be achieved only by |al or complete removal of the coating. The decontami)n test described gives a method of evaluating the five ease of decontamination of a coating system. The |sr the overall Decontamination Factor (DF), the easier ^coating will be to decontaminate. ;jgj J >Ki; lilU Dili few5 nsid atin| ating ! el Ilf anjj itmnfl con-- Physical Properties |Jl Adhesion--Panels shall be tested for adhesion in iprdance with Method D 4541. A minimum of two panels P be tested for each coating system. If the size of the test Ipmen is less than 3 in. by 5 in., an annular bearing ring Ijild be used to ensure full contact of the tester legs to the : specimen. j.l.I Minimum adhesion shall be 200 psi, consisting of : adhesion tests on each test panel. 1.2 Abrasion Resistance--Abrasion resistance characterisBof coating systems for floors and other surfaces where ffesionjs a factor shall be determined in accordance with It Method D 4060. jj|l2.1 Weight loss shall not exceed 175 mg/1000 cycles en a CS-ll Wheel is used with a 1000-g load. ! Chemical Resistance Tests 19.1 Test specimens shall be tested in accordance with Test jpthod D 3912. 19.2 The specific chemicals to be used should be selected to aracterize the anticipated exposure; the chemicals indi. in Test Method D 3912 are shown only as examples |d are not mandatory. atioil ; the, 2W0Z 1 Fire Evaluation Tests | 10.1 Flame Spread Tests--Flame-spread tests, when rered, shall be conducted and evaluated in accordance with Method E 84. The permissible flame-spread and smoke aeration, when tested on a noncombustible substrate, shall bt exceed the limits set by the nuclear power generating " :ility. 10.2 The coating systems should be tested to cover the specified film thickness range (or greater) since the flamespread and smoke density can yary "with film thickness. Smoke density is significant where a coating is utilized in . enclosed spaces and smoke generation, can reduce visibility and prevent effective fire fighting operations. Historic test data indicates that most coatings applied at less than 25 mils , dry film thickness over noncombustible substrates and tested in accordance with Test Method E 84 demonstrate flamespread values below 25. 11. DBA Testing 11.1 The test specimen shall be tested and evaluated in accordance with Test Method D 3911. 12. Surface Preparation, Coating Application, and Inspec tion for Shop and Field Work 12.1 It is recommended that the Manual ofCoating Work for Light-Water Nuclear Power Plant Primary Containment and Other Safety-Related Facilities Guide,7 prepared by ASTM Subcommittee DO 1.43, be reviewed in the course of nuclear coating work. 12.2 Surface preparation for steel, concrete, and previ ously coated surfaces shall be at least as good as that used in the qualification testing of the coating system intended for use. 12.3 Coating application shall be in accordance with the job specifications and the coating manufacturer's latest published instructions. Journeymen painter qualification shall meet the requirements of the applicable quality assur ance (QA) program. Practices D 4227 and D 4228. Coating dry film thickness shall be in the range used in the qualifica tion testing of the coating system. 12.4 Coatings work shall be inspected by coatings inspec tors qualified and certified in accordance with the applicable QA program and Guide D 4537. Inspections shall be docu mented to provide a record of the coatings work. 12.5 Maintenance painting work shall follow the require ments of 12.2, 12.3, and 12.4. The maintenance painting specifications shall take into consideration the plant environ ment in which the coating work must be accomplished. Maintenance painting work qualification testing should- be based on proposed surface preparation, coating application methods, and film thickness ranges, all of which may be different than the original design qualification work. 13. Quality Assurance 13.1 A quality assurance program for Service Level I coating work shall be established in accordance with Practice D 3843. Quality assurance requirements may also be estab lished for Service Level II coating work based on criticality. 14. Keywords 14.1 ANSI replacement standards; Design Basis Accident (DBA); decontamination; nuclear power plants; protective coating standards; qualification testing; quality assurance Service Level I and II; radiation; safety related 7 ASTM, 1979. DUP050298139 D 5144 TheAmerican Society for Testing and Materials takes no position respecting the validity oi any patent rights assertedin connection with any item mentioned In this standard. Users ol this standard are expressly advised that determination of the validity of any such patent rights, and the risk 61 Infringement of such rights, are entirety their own responsibility. This standard Is subject to revision atany time by the responsible technicalcommittee and must be reviewed every five years and If notrevised, eitherreapprovedor withdrawn. Your comments ere Invitedeither forrevision ofthis standardortor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have net received a fair hearing you should make your viewa known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 960 DUP050298140 Designation: D 5145 - 90 Standard Test Methods for Nonvolatile and Pigment Content of Electrocoat Baths1 This standard is issued under the fined designation D 5145; toe number immediately following the designation indicates toe year of original adoption or, in the case of revision, toe year of last revision. A number in parentheses indicates the year of last reapproval. \ superscript epsilon (> indicates an editorial change since the last revision or reapproval. pe i These test methods cover the characterization of ' coat baths through the determination of nonvolatile 'it of inorganic pigment content. I This standard does not purport to address the safety -ms associated with its use. It is the responsibility ofthe of this standard to establish appropriate safety and -practices and determine the applicability ofregulatory 'ations prior to use. Iferenced Documents ASTM Standards: jhl93 Specifications for Reagent Grade Water2 `832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings3 180 Practice for Determining the Precision Data of ; ASTM Methods for Analysis and Testing of Industrial iChemicals4 :L urmnary of Test Method ,1 Two specimens are accurately weighed into aluminum hing dishes. The dishes are placed in an oven at 1 iOC T h, reweighed to obtain the nonvolatile matter content , if required, placed in a muffle furnace at 500C for 2 h I weighed a third time to obtain the inorganic pigment lent. ]. {Significance and Use .1 The nonvolatile content and pigment content are insures of total solids and inorganic pigment solids, spectively, in electrocoat paints. In addition to production "lity control, these properties are important in mainning electrocoat baths in the optimum range. .4.2 Other test methods for determining nonvolatile con' t of paint and paint related materials are described in ethod D 2832. . Apparatus :5.1 Analytical Balance with a sensitivity of 0.1 mg. 5.2 Aluminum Weighing Dishes, 57 mm in diameter and 7 mm deep. These commercial dishes may contain a kbricant used during their manufacture. This should be `moved by heating the aluminum dishes on a hot plate at 1 These test methods are under the jurisdiction of ASTM Committee D*1 on .aim and Related Coating and Materials and are ihe direct responsibility of * 'bcommittee DO 121 an Chemical Analysis of Paints and Paint Materials. Current edition approved Dec. 13, 1990. Published January 1991. 2 Annual Book ofASTM Standards^ Vols 06.03 and 11.01. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vol 15.05. 300C until vapors are no longer visible. Store the dishes in a desiccator until needed. 5.3 Syringes, 5-mL, disposable'variety. 5.4 Oven circulating, maintained at 110 2C. 5.5 Muffle Furnace, maintained at 500 ' 15C. 6. Reagents 6.1 Purity of Water--References to water shall be under stood to mean water conforming to Type II of Specification Dim 7. Sampling and Sample Preparation 7.1 Obtain the sample while the electrocoat bath is under proper circulation so a uniform sample is obtained. In the case of a ultrafiltrate sample, the material should be thor oughly mixed or stirred prior to drawing the sample, thereby ensuring uniformity. 7.2 After sampling, prior to removing the test specimen, it is mandatory the sample be shaken or stirred until it is homogeneous and free of any settled material. This is particularly important if there is a delay between sampling the bath and performing this test procedure. The absence of settled material should be ascertained visually or by inserting a spatula and scraping the bottom of the container. Continue to shake or stir the sample until specimens are taken for measurement. This Point is Very Important. 8. Procedure MONVOLATILE CONTENT 8.1 Weigh two aluminum dishes separately, each to 0.1 mg and record as Wt. 8.2 Using a syringe, withdraw 1.0 to 1.5 of the well mixed sample, then quickly weigh the syringe to 0.1 mg, recording this weight as W2. Transfer the entire contents of the syringe into the aluminum dish. Reweigh the empty syringe to 0.1 mg and record as W3. In the case of ultrafiltrate clear liquids or of low solids paints, increase the specimen size to 5 mL and preheat at 60C for 2 h. Duplicate this step with the second aluminum dish (8.1). 8.3 Add a few millilitres of water to the specimen in the aluminum dishes prior to placing them in the oven. This facilitates uniform spreading of the material. Place the dishes in the 110"C oven for 1 h. 8.4 Remove the dishes from the oven and allow to cool to room temperature in a dessicator. Reweigh them to 0.1 mg and record the weights as WA. 8.5 Retain the dishes for measurement of inorganic pig ment content as detailed in a following section of these test methods. 961 DU P05 02 98141 9. Calculation 9.1 Calculate the percent nonvolatile content as follows: , NV = WA- W,`x 100 w2-w3 where: W- = weight of empty aluminum dish, g, W2 = weight of syringe filled with sample, g, fV3 = weight of empty syringe, g, and W4 = weight of dish and contents after I h at 110C, g. 10. Precision and Bias 10.1 Precision is based on an interlaboratory study in which the operators in each of ten laboratories analyzed in duplicate on 2 days, four different electrocoat-bath samples with nonvolatile contents ranging from 0.30 to 25.2 % The results were analyzed statistically in accordance with Practice E 180. The interlaboratory coefficient of variance was 1.6 % at 30 df and the interlaboratory coefficient of variation was 2.3 % at 21 df. Based on the these coefficients, the following criteria should be used forjudging the acceptability of results at the 95 % confidence level: 10.1.1 Repeatability: Two results, each the mean of dupli cate determinations obtained by the same operator on different days, should be considered suspect if they differ by more than 4.6 % relative. 10.1.2 Reproducibility: Two results, each the mean of duplicate determinations obtained by operators in different laboratories, should be considered suspect if they differ by more than 6.7 % relative. 10.2 No bias has been determined for this test method. 11. Procedure INORGANIC PIGMENT CONTENT 11.1 Place the weighing dishes used for the nonvolatile content determination in the muffle furnace at 500C for 2 h. 11.2 After 2 h, remove the dishes from the muffle furnace, transfer them to a dessicator and allow to cool to room temperature. After cooling, remove dishes and weigh to 0.1 mg, recording these weights at Ws. N;<' 1--If an organic char is still present in the aluminum dish aii' - 2 h in the muffle furnace, continue heating in the furnace until no ** is present. 12. Calculation 12.1 Calculate the percent inorganic pigment as follows i Inorganic Pigment (EC Bath) =- W, ~ - W, W, x 100 where: W, = weight of empty aluminum dish, g, W2 = weight of syringe filled with sample, g, = weight of empty syringe, g, and '' = weight of aluminum dish and contents after heating if in muffle furnace, g. 13. Precision and Bias 13.1 Precision estimates are based on ah interiaboratorv study in which the operators in ten different laboratories ' analyzed in duplicate on 2 days, four electrocoat bath materials containing inorganic pigment content ranging from 0.17 to 4.52 weight %. The results were anahzej statistically in accordance with Practice E 180. The intralaboratory coefficient of variation was 2.2 % relative at 40 df and the interlaboratory coefficient of variation wj, 10.8 % at 36 df. Based on these coefficients, the followine criteria should be used forjudging the acceptability of result at the 95 % confidence level: 13.1.1 Repeatability: Two results, each the mean of dupii cate determinations, obtained by the same operator on different days, should be considered suspect if they differ by more than 6.3 % relative. 13.1.2 Reproducibility: Two results, each the mean oi duplicate determinations, obtained by operators in different1 laboratories, should be considered suspect if they differ by more than 31.1 % relative. 13.2 No bias has been determined for this test method. 14. Keywords 14.1 electrocoat bath; muffle furnace; nonvolatile con tent; pigment content; ultrafiltrates |ope { _ i This! Resting I Ifior or bj _ can be, sedures i [OTE l--t ) Jpion i" I `Ipnary, ail Ifo intend SI, or indjpt feive ape' ll called T| fprE 2--|A fgrmancei^ iIi*n. ore stair?; |.2 The.t;, bllows:. I S) Type I) Type i fitnels, pa i|) Type; 'v jlered by t p) Types' lered bjjr'i 1.2.1 Epo |ayingv.pif i$e, which tt.jfel, preyii ;. icstrates. k The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination df (fie validity of any such patent rights, and the risk ot infringement of such rights, are. entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend, it you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. . Referent > .1 /isjlfc >16 te|.,, and Re| 93 Test; , Closedi? D154GC it) 185 ,T|. Pasles,S? {D2i5M(t Paints* I 1 This guide| jjlated Coatire pi.42 on Ard 3 Current edr z Annual Bi !lV3 Annual Bi |j * Annual Bi 7 . f 5 Annual B< * 962 jjgjlg ill DUP050298142 Designation: D 5146 - 90 "til no < Standard Guide to Testing Solvent-Borne Architectural Coatings1 This standard is issued under the fixed designation D 514S; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. er huatin4- iaboiatf i bni<.tor.i',-*`; coat , * ran^%l analj 180. I'm. relative^ ation following ' ofresult J of duplBga erator on* i differ bjf . m ean qf different differ n nethod MS atile con- I This guide covers the selection and use of procedures feting solvent-borne coatings to be used on exterior, gpr or both types ofsurfaces (see Note 1). The properties ban be examined or, in some cases, the relevant test Idures are listed in Tables 1 and 2. ijrE 1--The term "architectural coating" as used here combines the Sion in Definitions D 16 with that in the FSCT Paint/Coatings linary, as follows: "Organic coatings intended for on-site applica- |> interior or exterior surfaces of residential, commercial, institu[, or industrial buildings, in contrast to industrial coatings. They are live and decorative finishes applied at ambient temperatures. U called Trade Sales Coatings." (See 2.3.). IS=' 2--Architectural coatings that are designed to give better rinance than most conventional coatings because they are tougher non: stain- and abrasion-resistant are covered by Guide D 3730. (g The types of organic coatings covered by this guide are bllows: It) Type 1 Interior Low-Gloss Wall Finish, partly covered fgjuide D 3323, |) Type 2 Interior Gloss and Setnigloss Wall and Trim pnels, partly covered by Guide D 342.5, gj Type 3 Exterior House and Trim Coatings, now red by Guide D 2932, and Jft) Type 4 Floor Enamel, Exterior and/or Interior, now ||ered by Guide D 3383. |i2.1 Each is intended for application by brushing, rolling, lying, or other means to the materials appropriate for its b, which may include wood, plaster, wallboard, masonry, Jbl, previously painted surfaces, and other architectural pstrates. eferenced Documents 2.1 ASTM Standards: 116 Terminology Relating to Paint, Varnish, Lacquer and Related Products2-3-4 |D93 Test Methods for Flash Point by Pensky-Martens . Closed Tester5 jfp 154 Guide for Testing Varnishes2 lib 185 Test Methods for Coarse Particles in Pigments, Pastes, and Paints2-3 ' D 215 Methods of Chemical Analysis of White Linseed Oil p Paints2 v||1 This guide is under the jurisdiction of ASTM Committee D-l on Paint and plated Coating and Materials and is the direct responsibility of Subcommittee pH .42 on Architectural Finishes. fi Current edition approved Nov. 30, 1990. Published January 1991. 1i2 Annual Book ofASTM Standards, Vol 06.01. %} Annual Book ofASTM Standards, Vo! 06.02. si 4 Annual Book ofASTM Standards, Vol 06.03. I; s Annual Book ofASTM Standards, Vols 05.01, 06.01, and 06.03. D344 Test Methods for Relative Hiding Power of Paints by the Visual Evaluation of Brushouts2 D358 Specification for Wood to be Used as Panels in Weathering Tests of Coatings2 D522 Test Method for Mandrel Bend Test of Attached Coatings2 D523 Test Method for Specular Gloss2 D 562 Test Method for Consistency of Paints using the Stormer Viscometer2 D 658 Test Method for Abrasion Resistance of Organic Coatings by Air Blast Abrasive2 D659 Test-Method of Evaluating Degree of Chalking of Exterior Paints2 D 660 Test Method for Evaluating Degree of Checking of Exterior Paints2 D 661 Test Method for Evaluating Degree of Cracking of Exterior Paints2 D662 Test Method for Evaluating Degree of Erosion of Exterior Paints2 D772 Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints2 D 968 Test Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive2 D 1006 Practice for Conducting Exterior Exposure Tests of Paints on Wood2 D 1014 Test Method for Conducting Exterior Exposure Tests of Paints on Steel2 D 1038 Definitions of Terms Relating to Veneer and Plywood6 D 1208 Test Methods for Common Properties of Certain Pigments3 D 1210 Test Method for Fineness of Dispersion of Pig ment-Vehicle Systems2 . D 1296 Test Method for Odor of Volatile Solvents and Diluents4 D 1308 Test Method for Effect of Household Chemicals on Clear and Pigmented Organic Finishes2 D1475 Test Method for Density of Paint, Varnish, Lac quer and Related Products2 D 1543 Test Method for Color Permanence of White Architectural Enamels2 D1554 Definitions ofTerms Relating to Wood-Base Fiber and Particle Panel Materials6 D 1640 Test Methods for Drying, Curing or Film Forma tion of Organic Coatings at Room Temperature2 D 1729 Practice for Visual Evaluation of Color Differences of Opaque Materials7 6 Annual Book ofASTM Standards, Vol 04.09. 7 Annua! Booh ofASTM Standards, Vo) 14,02. DU P050298143 D 5146 D 1849 Test Method for Package Stability of Paint2 D2196 Test Methods for Rheological Properties of Non- Newtonian Materials by Rotational (Brookfield) Viscometer2 D 2197 Test Method for Adhesion of Organic Coatings by Scrape Adhesion2 D 2244 Test Method for Calculation of Color Differences from Instruihentally Measured Color Coordinates2 D 2245 Method for Identification of Oils and Oil Acids in Solvent-Reducible Paints4 D 2369 Test Method for Volatile Content of Coatings2 D2370 Test Method for Tensile Properties of Organic Coatings2 D2371 Test Method for Pigment Content of Solvent- Reducible' Paints2 D2372 Method of Separation of Vehicle from Solvent- Reducible Paints2 D 2486 Test Method for Scrub Resistance ofInterior Latex Flat Wall Paints2 D2621 Method for Infrared Identification of Vehicle Solids from Solvent-Reducible Paints2 D2697 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings2 D2698 Method for Determination of the Pigment Con tent of Solvent-Reducible Paints by High Speed Cen trifuging2 D2805 Test Method for Hiding Power of Paints by Reflectometry2 D2932 Guide for Testing Exterior Solvent-Reducible House and Trim Coatings2 D3278 Test Methods for Flash Point of Liquids by Setaflash Closed Apparatus4 D 3323 Guide for Testing Interior Solvent-Reducible Flat Wall Paints2 D3359 Test Methods for Measuring Adhesion by Tape Test2 D3383 Guide for Testing Solvent-Reducible Floor Paints2 D3425 Guide for Testing Solvent-Reducible Interior Semigioss Wall and Trim Enamels2 D 3450 Test Method for Washability Properties of Interior Architectural Coatings2 D3456 Practice for Determining by Exterior Exposure Tests Susceptibility of Paint Films to Microbiological Attack2 D3730. Practice for Testing High-Performance Interior Architectural Wall Coatings2 D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings2 D3928 Test Method for Evaluation of Gloss or Sheen Uniformity2 D4017 Test Method for Water in Paints and Paint Materials by Karl Fischer Method2 D4060 Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser2 D4062 Test Method for Leveling of Paints by Draw-Down Method2 D4213 Test Method for Wet Abrasion Resistance of Interior Paints2 D4214 Test Methods for Evaluating Degree of Chalking of Exterior Paint Films2 D4287 Test Method for High Shear Viscosity of and Varnishes by the IC1 Cone/Plate Viscometer ;1 D4400 Test Methods for Sag Resistance of Paints Using#* Multi notch Applicator2 D4585 Practice for Testing Water Resistance of Coa ; Using Controlled Condensation2 D4707 Test Method for Measurement of Paint Sp Resistance to Roller Application2 D4828 Test Method for Practical Evaluation of Wa$|r ability of Organic Coatings2 "f E 97 Test Method for Directional Reflectance Factor^ 45-deg 0-deg, of Opaque Specimens by Broad-B mjL Reflectometry8 n v' E 105 Practice for Probability Sampling of Materials E 313 Test Method for Indexes of Whiteness and Yellow^ ness of Near-White Opaque Materials7 'J 2.2 US. Federal Standard: U.S. Federal Test Method Standard No. 14189 2112 Application by Roller . 2131 Application of Sprayed Films 2141 Application of Brushed Films 3011 Condition in Container 4203 Reducibility and Dilution Stability 4401 Odor Test 4421 Absorption Test 4541 Working Properties and Appearance of Dried Film * 2.3 Other Document: Paint/Coatings Dictionary of the Federation of Societies!) for Coatings Technology10 3. Terminology 4`J3.1 For definitions of terms in this guide refer to Defini tions D 16, D 1554 and D 1038 and to the FSCT Pm:. Coatings Dictionary. 4. Conditions Affecting Solvent-Reducible Coatings 4.1 Substrate Type--The substrate to be painted . n affect not only the application properties of a coating, such as gloss and uniformity, but is also a factor in determining '.I >. type ofcoating to use. For instance, low-gloss wall finishes do not have the abrasion resistance required on floors, -whereas finishes intended only for interior service probably do not have adequate resistance to weather factors. Other, factors are the type and quality oFwood or wood composite (plywood, particle board or hardboard), the type, quality and alkaline of concrete, plaster and joint cement systems, and the type and condition of any previous coatings. 4.2 Substrate Conditions--Conditions such as porosity, hardness or, in the case of unpainted concrete, alkalinity determine the kind of coating that can be applied. The condition of previously painted substrates, such as degree of chalk, presence of grease, dirt, and mold, film adhesion and porosity, and the general condition of the previous coating, all influence the performance of coatings. Smoothness of the substrate affects the spreading rate, final appearance, and texture. 4 8 Annual Book ofASTM Standards, Vols 06.01 andI4.02. 9 Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 191U-5094. 10 Available from the Federation of Societies for Coatings Technology, 492 Norristown Rd., Blue Bell, PA 19422. 964 DUPO 50298144 D 5146 TABLE 1 leter Ms Usijj|! jtv 1 So Property (or related test) gPaint Properties lining pdltian in container int Spat) jirse particles and foreign matter felly or Weight per gallon finess of dispersion f Hasip' :e Facto/., raad-Banjjj'l insistency jjfeological properties of non-Newtonian liquids pi point for [sorption iilorant acceptance srials7. sjS jjtion stability Stage stability pig Application and Film Formation Implication properties ^jish appKcation i&fler application jfoBer spkter pay application ing properties .jvellng properties ||ag resistance ipuch up uniformity Jarance of Dry Flm Jolor difference by visual comparison iplor difference by instrumental measurement sd Film Jptectional reflectance Gloss floss, 60 Societies V* iheen (85gloss} piding power "pilowness index > Deflni.?* ' Pami' parties of Dry Film Bfnterior and Exterior Coatings jp Abrasion resistance jjii Adhesion K. Flexibility ^Interior Coatings HI Color change of while enamels :ed ,,an,-i such.iv* mk Washability arid cleansability S|. Washabillty m" Cleansability W Resistance to household chemicals ling the shesdo vhere<.,v do not f;l pExterior Coatings w- Blister resistance ft Exposure resistance m Chalking H Checking tors me , ywooc. T* taliniti te type p Cracking ft Erosion I Flaking I- Mildew resistance 1 Fume resistance loatlng Analysis TOSil s alinjt> | Coating analysis i Volatile content If. Nonvolatile volume content I. Th" tree of <n and lating, of the jfWater content , Pigment content t* Pigment analysis j? Nonvolatile vehicle content Vehicle separation : Nonvolatile vehicle identification anr. A Equivalent only to Method B of Test Method D 522. B Except for scrub medium. c 6271 is not equivalent. List of Standards in Sectional Order Section ASTM Standard 6.2 D3925 7.1 7.2 7.3 7.4 7.5 7.6 7.7 7.8 7.9 7.10 7.11 7.12 7.13 8.1 8.1.1 8.1.2 8.1.2.1 8.1.3 6.2 8.3 8.4 8.5 D154 D185 D1475 D1210 D 562 D 2196,D 4287 D 93. D 3278 D 1296 D1849 D4707 D 1640 D 4962 D 4400 D3928 9.1 9.2 9.3 9.4 9.4.1 9.4.2 9.5 9.6 D1729 D2244 E 97 D 523 D523 D 344, D 2805 E 313 10.1 10.1.1 10.1.2 10.1.3 10.2 10.2.1 10.2.2 10.2.2.1 10.2.2.2 10.2.3 10.3 10.3.1 10.3.2 10.3.2.1 10.3.2.2 10.3.2.3 10.3.2.4 10.3.2.5 10.3.3 10.3.4 D 658, D 960. D 4060 D 2197, D 3359 D 522, D2370 D 1543 D 2486. D 4213 D 3450. D 4828 D 1308 D 4585 D 1006, D 1014 0 659, D 4214 0 660 D 661 D 662 D 772 D 3456 11.1 11.2 11.3 11.4 T1.5 11.6 11.7 11.8 11.9 D 215 D 2369 D 2697 D 1208, D 4017 D 2371 D 215 D 215 D 2372 D 2621. D 2245 Federal Test 1 Standard 1022 3021 3011 4401 4421 4203 4541 2141 2112 2131 4061 4494 6131 6192 6221' 6192' 614V 4081 4021 7261 4053 Wwk. jj| 4.3 Substrate Aspects of the Building--If construction (Prefects or defects due to age are such that excessive moisture the inside or the outside makes its way through the substrate or if the substrate is in direct contact with damp ground, blistering, flaking or peeling may result. 4.4 Preparation of previously painted substrates including 965 DUP050298145 # D5146 Property (or related test) Abrasion Resistance Absorption Adhesion Analysis Application properties Brush application Chalking Checking C/eansabfllty Coarse particles and foreign matter Colorant acceptance Color change Color difference by instrumental measurement Color difference by visual comparison Condition in container Consistency Cracking Density or weight per gal Dilution stability Drying properties Erosion Fineness of Dispersion Flaking Flash point Flexibility Fume resistance Gloss Gloss, 60 Hiding power Levelling properties Mildew resistance Nonvolatile vehicle content Nonvolatile vehicle identification Nonvolatile volume content Odor Package stability Pigment analysis Pigment content Resistance to household chemicals Rheological properties of non-Newtonian liquids Poller application Roller spatter Sag resistance Sampling Sheen (85 gloss) Skinning Spray application Touch up uniformity Vehicle separation Volatile content Was liability Water content Yellowness index A Except for scrub medium. a Equivalent only to Method B of D 522. c 6271 is not equivalent. ' TABLE 2 Alphabetical' List of Properties Section ASTM Standard l f ,, 10.1.1 7.10 10.1.2 11.1 8.1 8.1.1 10.3.2.1 ` 10.3.2.2 10.2.2.2 7.3 7.11 10.2.1 9.2 9.1 7.2 7.6 10.3.2.3 7.4 7.12 8.2 10.3.2.4 f 7.5 10.3.2.5 7.8 10.1.3 10.3.4 9.4 9.4.1 9.5 8.3 10.3.3 11.7 11.9 11.3 7.9 7.13 11.6 11.5 10.2.3 7.7 8.1.2 8.1.2.1 8.4 6.2 9.4.2 7.1 8.1.3 8.5 11.8 11.2 10.2.2.1 11.4 9.6 D 658. D 968, D 4060 D 2197,0 3359 D 215 D 659, D 4214 D660 D 3450, D 4828 D 185 D 1543 0 2244 D 1729 D 562 O 661 D 1475 D 1640 0 662 D 12^0 D772 D 93, D 3278 D 522, D2370 D 523 D 344, D 2805 D4062 D 3456 D 215 D 2621, D 2245 D 2697 D 1296 D1849 D 215 D 2371 D 1308 D2196, D 4287 D 4707 D 4400 D3925 O 523 D 154 D 3928 D2372 D 2369 0 2466,0 4213 D1208. D4017-----' E 313 Federal Test ii Standard 141 V' t `C.S 'Ll' 6192 4421 ~ "--e '-A jpggLuy jilt'd 4541 2141 < 6141** ' 8192 JjgthTlS tflV -i i 3021 'W&uae 4203 4061 6221 c 4053 4401 7261 4021 2112 4494 1022 3021 2131 4061 6131 <}1 rillld* * smrifri a m'V.n 3 1 H tfblu 1 ii v i if,3 $ u Bp V IV 1 tut i id Tii1 'G C -p ' f wgpu1 mnh ti T.dns, \*tfn-lr rjbiAi'icl ? 1 detergent cleaning, solvent cleaning, and sanding. 4.5 Type, and quality of primer or undercoat and time of drying before topcoating. 4.6 Environmental conditions such as temperature and humidity at the time of coating application and during drying. 4.7 Environmental conditions after application, both gen eral for the area and specific, such as under eaves, behind shrubbery, northside and southside exposure.5 5. Selection of Tests 5.1 Because the conditions to which a coating is subjected vary with (a) the surface type: wall, floor, ceiling, and {b) the service environment: exterior or interior, specialized types ol solvent-borne coatings have been developed for the different locations. The recommended test methods presented i'r Tables 1 and 2 cover practically all the properties ol solvent-reducible coatings but all of them are not required with each type. Coatings intended for exterior use only 01 both exterior and interior use require certain properties not relevant to those for interior use only. Selection of the methods to be followed must be governed by experience and the requirements in each individual case, together with agreement between the purchaser and the seller. 5.2 The purchaser should first determine the properties a coating should have and then select only those test methods 966 DUP050298146 ;ypes of ifferent ited in ties of squired only or :ies not of the ice and t with srties a ethods # D 5146 neasure or evaluate those properties. After selecting the l tests, the purchaser should then decide which propare the most important and establish the requirements deifications accordingly. Since coating properties frepy tend to oppose each other, such as low sheen versus Ifcleansability, some properties may need to be less iasized if others are to be accentuated. This balance of ties must be considered when selecting the tests and {fishing the requirements. The significance of the tests he normal range of values are presented in the different |tas, in most cases. This guide does not indicate relative importance ofthe ps tests nor does it recommend specific test values use properties very important to one purchaser may be i to another. |mpling Prior to sampling, the condition of the container I'd be checked since damage to it may cause evaporation, png, or other undesirable effects on the coating. Sample in accordance with Practice D 3925. Deterthe density in pounds per gallon (kilograms/litre)' in ifdance with Test Method D 1475. Continue sampling determining density until successive results agree within i (45 g) or as agreed upon between the purchaser and , Then take samples for testing. Specify the amount requited for a representative ble, the package sizes, and an identification- code. A {gS. gal (or 4-L) sample is usually sufficient for the amended tests, but for guidance in selecting a sampling |consult Practice E 105. liquid Coating-Properties R Skinning--Coatings that contain a binder that dries Sedation may be subject to skin formation in a partially- 1 can: Since skins are insoluble in the material they must jjemoved before use. The referenced test in a partially- container indicates the tendency of the material to a. A typical minimum time for skinning in accordance V this method is 48 h. Examine the original sample for |s, both on and below the' surface. Using a well-mixdd glftee portion of the sample, perform a skinning test in Jfdance wtih Guide D 154. II Condition in Container--Thickening, settling, and aration are undesirable and objectionable if material that (been stored cannot be readily reconditioned and made able for application with a reasonable amount of stirring. ' referenced method covers procedures for determining nges in properties after storage and lists characteristics are undesirable and objectionable in a stored paint, iermine condition in the container in accordance with Shod 3011 of Federal Test Method Standard No, 141`. Sse also 7.13, Package Stability.) '.3 Coarse Particles and Foreign Matter--Liquid coatings gst be free of coarse particles and foreign matter to be able jjbnn uniform films of good appearance, a typical max im being 0.5 weight % of the total material. The srenced method with a 325-mesh (45-um) screen gives the jjpent of these, particles. Determine content of coarse Seles and foreign matter in accordance with Test Ihods D 185. 7.4 Density or Weight per Gallon--The density measured in pounds per gallon (kilograms per litre = g/mL) is used to ensure product uniformity from batch to batch, provides a check agaihst the theoretical weight calculated from the formula, and is useful for determining the similarity of two samples. The referenced method gives a procedure for measuring the density of the coating at a specified tempera ture. Most interior paints have densities of about 10 to 12 Ib/gal (1.2 to 1.4 kg/L). Determine density in, accordance with Test Method D 1475, using a calibrated weight per gallon cup. 7.5 Fineness ofDispersion--Generally, the more finely a pigment is dispersed, the more efficiently it is being utilized. One method for measuring the degree of dispersion (com monly referred to as "fineness of grind") is-to drdw the liquid coating down a calibrated tapered groove varying in depth from 4 to 0 mils (100 to 0 jxm) (0-8 Hegman units). The depth at which continuous groupings ofparticles or agglom erates, or both, protrude through the surface of the wet film is taken as the fineness of dispersion value: Higher readings in Hegman units or lower readings in mils or micrometres indicate finer dispersion. Low sheen finishes may have a dispersion value of.2 mils (50 pm or 4 Hegman) while gloss enamels might be neax zero (8 Hegman) indicating that the pigment agglomerates are too small to Be detected by the referenced method. Determine fineness of dispersion in accordance with Test Method D 1210. 7.6 Consistency (Low-Shear Viscosity)--Consistency is important, relating to application and flow, and should fall within a' stated range for satisfactory reproduction of a specific formula. While consistency is an important property it does not determine the quality of a coating and should be used mainly to ensure product uniformity. In the referenced method, consistency is defined as the load in grams to produce a specified rate of shear. The load.value is frequently converted to Krebs units (KU) and the Stormer Consistency reported on that basis. Although the consistency of most solvent-borne house and trim coatings is about 150 to 3Q0 g/100 revolutions (72 to 95 KU), a much wider range is possible because of the great variation that may occur in the rheological properties of these, paints. Enamels for profes sional painters are usually formulated at a higher consistency range than consumer enamels. Typical ranges are_75 to 90 KU Fox consumer enamels and 90 to 100 for professional painter'enamels. Two paints of the same consistency may have quite different rheological properties during applica tion. Determine the consistency in accordance with Test Method D 562. : 7.7 Rheological Properties ofNan-Newtonian Materials-- Rheological properties are related to application and flow characteristics of the liquid coating. The referenced methods cover the determination of rheological properties and are particularly suited for coatings that display thixotropic char acteristics. They actually measure viscosity under different shear rates. In Test Method D 4287 the rate is similar to that occurring during brush application so that the measured viscosity is related to brush drag, spreading rate and film build. Determine rheological properties in accordance with Test Methods D 2196 or D 4287, or both. 7.8 Flash Point--Organic solvents used in these coalings have characteristic temperatures at which they support DUP050298147 ii combustion. This temperature is known as the flash point and is often used for danger classification in shipping by common carrier. It is also used to determine conditions of storage to meet fire regulations and the safety requirements of the U.S. Occupational Safety and Health Act (OSHA). Determine flash point in accordance with Test Methods D 93, Part B, or D 3278. 7.9 Odor--Some solvent combinations produce obnox ious odors, particularly when painting indoors with inade quate ventilation and at elevated temperatures. Interior solvent-borne coatings usually contain low-odor or odorless mineral spirits. Nevertheless they should be evaluated to ensure that they are acceptable. Test for odor in accordance with Method 4401 of Federal Test Method Standard No. 141. Although not specifically designed for liquid coatings Test Method D 1296 may be used with the solvent-reducible type. 7.10 Absorption--On porous surfaces, binder penetration can result in pigment volume concentration changes as the film dries. This may cause appearance to vary. The refer enced method provides a rough measure of the wetting and penetrating properties of the binder on a porous surface. Determine the absorption in accordance with Method 4421 of Federal Test Method Standard No. 141. 7.11 Colorant Acceptance--Tintability ofwhite bases with colorants of standardized tinting strength is a trade require ment. If tinting colors are not adequately compatible with tint bases, lighter, darker, or nonuniform shades ofcolors are produced. There is no accepted ASTM test method at present. Test methods may be agreed upon between the purchaser and seller. 7.12 Dilution Stability--Dilution with a specified thinner shows whether the materials are compatible and whether the reduced coating is stable. Consequently the suggested diluent should be readily incorporated into the coating without excessive stirring or shaking. The referenced method evalu ates the stability of the' material that has been reduced by a giveh amount or to a specified viscosity. Determine dilution stability in accordance with Method 4203 of Federal Test Method Standard No. 141. 7.13 Package Stability--Since paints cannot normally be used immediately after manufacture, they must remain stable in the can for some time. At normal temperatures most paints can be stored'for over a year with little change in properties. Although indications of long term package sta bility can usually be obtained in several days or weeks'at an elevated temperature, such as 122F (50C) or 140F (60"C), occasionally the results of the accelerated test do not agree with those at prolonged normal storage conditions. The referenced method predicts the change in consistency and certain other properties of packaged paint when stored at temperatures above freezing. Determine package stability in accordance with Test Method D 1849. 8. Coating Application and Film Formation 8.1 Application Properties--Application or working prop erties of a paint are generally compared to a standard or described by requirements in the product specification. Determine working properties in accordance with Method 454! of Federal Test Method Standard No. 141. 8.1.1 Brush Application--Brushed films should be smooth and free of seeds and on vertical surfaces should I show no sagging, color streaking, or excessive brush mark^ff Brush drag should not be excessive although some degrefr'Jii drag may be desirable for adequate film thickness appi^;^* tion. Wall finishes are tested on vertical surfaces and enamels on horizontal surfaces, although evaluation of th/'sl latter on vertical surfaces may be necessary to determine^*'* performance on stair risers, railings, posts, etc. The refer. \ enced method covers a means for the determination oi i)5tr" brushing properties of a coating. Even though the tes: ^ subjective someone experienced in the art can produce quite consistent results, particularly in the evaluation of drai "'.i qualities. Determine the brushing properties in accordance with Method 2141 of Federal Test Method Standard \o 141. 8.1.2 Roller Application--Both wall and floor coating- Jrc frequently applied by roller. This type of application tends to produce some stipple pattern. The referenced method covers the evaluation ofa material's characteristics when applied > > roller. Determine roller coating properties in accordance with Method 2112 of Federal Test Method Standard No, 141. 8.1.2.1 Some coatings spatter more than others when applied by roller. The degree to which a paint spatters when roller applied can be determined by the density ofthe spauer. In the referenced method a specially designed notched sped is rolled through a film of the test material that has been applied to a plastic panel. Any spatter generated fells upon i catch paper and after drying is rated against photographic standards. This procedure eliminates the influence of the, roller cover, thus determining the spattering characteristic of the paint alone. Determine spatter resistance in accord ance with Test Method D 4707. 8.1.3 Spray Application--Architectural coatings are sometimes applied by spray. Both air and airless .spray are used on commercial work. Determine the spray application properties in accordance with Method 2131 of Federal 'Usi Method Standard No. 141. Manual application is very, subjective and should be performed only by an individual skilled in the art of using spray equipment. 8.2 Drying Properties--The drying time of a coating is important in determining when a freshly painted room, floor or stair may be put back in use. Slow drying may result in dirt or insect pickup resulting in a poor appearance or, ii -t an exterior surface, rain or dew may cause a nonuniform appearance. The drying time ofa coating is determined by us composition and by atmospheric conditions during drying. Typical drying times for enamels are 'A to 2 h set-to-touch and 18 h dry hard under normal temperature and humidity conditions. Some coatings lose drying speed during storage in the container. Any of the several methods for determining the various stages of film formation in the drying or curing of organic coatings may be used. For example, if two coats are specified the determination of "dry-to-recoat" time is impor tant. Determine appropriate drying timefs) in accordance with Test Methods D 1640. 8.3 Levelling Properties--Levelling is an important prop erty when smooth, uniform surfaces are to be produced, as it affects hiding and appearance. The referenced method covers the relative levelling characteristics of liquid coatings. Deter mine levelling in accordance with Test Method D 4062. 8.4 Sag Resistance--Some coatings sag and form curtains acce. spec?; Jlasf loaf. 968 DUP050298148 1 marks., iegrce of! aPlMcaj, 'a fore the film sets. This is an important property particufly for semigloss and gloss enamels because sagging results (unsightly film appearance. Measure sag resistance in ordance with Test Methods D 4400. ao`'th^J ^icnnineM le refejj-BjL n of tfti ** 5 tesi is*" CetJUtiiSa of dragS'-l ordancc rrd N0f fid Touch-Up Uniformity--After a paint has dried, areas re less material was applied sometimes become noticeE), If the paint has suitable touch-up properties, additional jgterial can be applied to these areas only, instead of fishing the complete wall. The color, gloss, and levelling jjphe touched-up areas and the previously coated area jktld be uniform. Differences in these properties are often feed by short wet-edge time, poor levelling on recoat, and gment orientation or flotation during and after application. Pennine touch-up properties in accordance with Test ings ate'(3 ithod D 3928. tends to AS i covers'll ^Appearance of Dry Film plied by <3 ,1 Color Differences by Visual Comparison--Visual 3rdance3SI mparison of colors is fast and often acceptable although ird Imerical values are not obtained. The referenced method s nhen. rs when; spatter,! pers the spectral, photometric, and geometric characteris es oflight source, illuminating and viewing conditions, sizes {specimens, and general procedures to be used in the visual {aluation of color differences of opaque materials relative to d spool; ` as been'upon a graphiCffe of %fs tei ivies. ,* accorjiiH |eir standards. Determine color difference in accordance fth Practice D 1729. 1.2 Color Differences Using Instrumental Measure ments--The difference in color between a product and its findard can be measured by instrument. Generally the lerance is agreed upon by the purchaser and seller and may be required if a product specification is involved. .Color is ate '< ray .ire'V licatinn. 1 al Test/J is very * ` li' dual ,, J tsuring instruments provide numerical values that can be ipared to subsequent measurements. The referenced Ipthod covers the calculation of instrumental determinams of small color differences observable in daylight illumi|tion between nonfluorescent, nonmetameric, opaque sur- Ipes such as coated specimens. If metamerism is suspected, isual evaluation (9.1) should be used to verify the results. iting iSjj? a, floor, ;sult in r, if on niform d by its drying t-touch imidity storage mining iring of* *ats areif| imporrdance * Iculate in accordance with Test Method D 2244 the color Terences that have been measured instrumentally. 9.3 Directional Reflectance--This property is a measure if the appearance of lightness of a coating. It is usually Ssigned a value in specifications for white and pastel shades, Etypicai minimum, reflectance value being 86 % for white iall paint. In the referenced method the directions of fumination and viewing are specified so as to eliminate the feet of gloss. Determine daylight directional reflectance in Pgcordance with Test Method E 97. 9.4 Gloss--This property is a measure of the capability, of , coating surface to reflect light in a mirror-like (specular) tanner, that is, light strikes the surface and is reflected at the Iqual but opposite angle. In the referenced method the Numerical gloss units are the ratio of light reflected by a specimen to that reflected by the primary standard black lass that is assigned a gloss value of 100. The gloss of some t prop floatings varies greatly with the angle of incidence so that a el, as it Ipmplete description of their gloss would require measure- covers tents over a wide range of angle. In practice, the gloss of Deter- rchitectural finishes is adequately characterized by measure- >2. ;>:d attains ! tents at 60 or 85, or both, from a line perpendicular formal) to the surface. The 85 angle is a very low ("grazing") angle (5) of illuminating and viewing the surface and the gloss at this angle is called "sheen". Attempts to standardize the levels of gloss associated with the several descriptive terms have not been very successful since the gloss scale is. continuous with no distinct boundaries. Hence, there is some overlap at the ends of some gloss classifications in common usage. 9.4.1 Gloss, 60--Semigloss enamels are particularly sen sitive to enamel hold-out of primers and undercoats. Low or uneven gloss readings are indicative of this defect. Oil house paints are typically in a 60gloss range from 30 to 70 while trim enamels are from 70 to 90. Floor enamels generally have a high (90+) gloss reading when first applied but this decreases- with time and traffic. Interior senaigloss enamels after drying 48 h are typically in the range from 40 to 70 but measurements taken shortly after drying should be repeated after one week because the gloss can drop considerably in the first few.days of drying. Determine the 60 gloss in accord ance with Test Method D 523. 9.4.2 Sheen (85 Gloss)--Although low-gloss paints with good uniformity ofappearance at low angles of viewingoften have little sheen while those with good cleansability usually have moderate sheen, this is not always the case so that sheen should not be used as a measure of other paint properties. Most flat wall paints have a sheen of about 1 to 10. The referenced method, using the 85 geometry, is useful in characterizing the low-angle appearance of low-gloss coat ings. Determine the sheen (85gloss) in accordance with Test Method D 523. N>?' 3--This property is of particular interest with flat to low-gloss finishes. 9.5 Hiding Power--Hiding power is a measure of the ability of a coating to obscure the substrate and is usually expressed as tshe spreading rate for a specified-- level of opacity. It is, however, dependent on uniformity of film thickness, which in practical applications is influenced by flow, levelling and application properties of the coating.-,Test Method D 2805 is precise and gives an absolute rather than a comparative result. Paint is applied with an applicator bar to minimize the effects of flow and levelling, film thickness is rigorously measured, and film opacity is determined instru mentally, Test Method D 344 is a practical test in which paint is applied with a brush, wet-film thickness is approxi mately controlled by spreading rate, and hiding power is evaluated visually by comparison with a standard paint, but resu.lts are affected by flow and levelling of the materials. Determine hiding power in accordance with Test Methods D 344 or PJ2805. 9.6 Yellowness Index--The referenced method is used for white or near white specimens to determine color departure from white toward yellow when first applied. Determine the yellowness index in accordance with Method E 313. (See also 10.2.1.) 10. Properties of the Dry Film 10.1 Interior and Exterior Coatings: 10.1.1 Abrasion Resistance--Abrasion resistance is a measure of the ability of a dried film to withstand wear from foot traffic and marring from objects rolled or pulled across D 5146 the surface. In the referenced methods, dry abrasive is applied to a coated panel using the force of gravity or a jet blast for free-flowing abrasive or a weighted wheel for abrasive embedded in a resilient rubber matrix. Determine dry abrasion resistance in accordance with Test Methods D 658, D 968 or D 4060. (See 10.2.2.1 for wet abrasion resistance.) N@A' 4--Because of the poor reproducibility of abrasion test methods, testing should be restricted to only one laboratory when numerical abrasion resistance values are to be used. Interiaboratory agreement is improved significantly when rankings are used in place of numerical values. 10.1.2 Adhesion--Adhesion is the property of a film that resists removal from the substrate. It is an important property in a paint. Determine adhesion in accordance with Test Method D 2197 or D 3359, or both. 10.1.3 Flexibility--Elongation is a measure of the flexi bility of a coating film. Generally, gloss house paints and trim enamels have no problems in passing a mandrel bend test at '/s in. (3.2 mm). However, interior flat and eggshell finishes may pass only a '/2-in. (12.7-mm) bend. For exterior coatings Test Method D 2370 is a much more discriminating method.11 Determine flexibility in accordance with Methods D 522 or elongation with D 2370. 10.2 Interior Finishes: 10.2.1 Color Change of White Architectural Enamels-- Color permanence is an important characteristic for interior white enamels. Lack of permanence is usually caused by after-yellowing. The referenced method attempts to accel erate color change by exposing coatings to dry sulfur dioxide. Determine resistance to color change in accordance Test Method D 1543. 10.2.2 Washability and Cleansability--The capability of satisfactorily removing marks without damaging the film is essential for good performance of interior finishes. A coating may be washable, that is, unaffected by the detergent solution, but may not have good cleansability. Frequently the difference between the two terms "cleansability" and "washability", is not clearly understood so that there is confusion as to what is really being tested; for example, the title of Test Method D 3450. Cleansabifity is evaluated by applying one or more stains and soils and determining how readily they are removed. Washability is evaluated by determining the resistance of the film to wet erosion either by visual assessment or measured film loss. In general, the precision of both types of test is poor because several properties, such as hardness, water and detergent resistance, cohesion and adhesion, are involved and the end point, except for the wet abrasion method, is rather indefinite. 10.2.2.1 Washability (Also referred to as Scrubbing or Wet Abrasion Resistance)--The scrubbing method, Test Method D 2486, developed for interior latex flat wall paints can be applied to coatings of almost any type. In it the coating is applied to a black plastic panel that, during scrubbing with a nylon brush and abrasive cleaning agent, is raised by a narrow shim to concentrate the test area. The number of back-and-forth strokes (cycles) required to remove the film over the shim is determined. The wet-abrasion method, Test u H. E. Ashton, Journal ofCoatings Technology> Vol 51, June 1979, p. 41. Method D4213, is similar except that a sponge is used irf' place of the bristle brush while the shim is not used. Thi|T method also provides for the use of a nonabrasive medium with paints having very low abrasion resistance. The weight or volume loss per 100 cycles to erode the film almost to exposure of the black substrate is the measure of scrub'-1 resistance. Evaluate washability, as described just, in accord- ? ance with Test Methods D 2486 or D 4213. 10.2.2.2 Cleansability--The older referenced methrd. Test Method D 3450, is similar to the wet-abrasion method^ Test Method D4213, except that the sponge is used with' either the nonabrasive or abrasive cleaning agent to remove a- carbon black-oil stain. The ability to remote the stain i&, expressed as the ratio (in percent relative) of the reflectance of the cleaned area to that of the area before application of the stain. In Test Method D 4828, referred to as a "practii nl ' test, numerous staining and soiling agents found in service and commercial abrasive or nonabrasive cleaners as well as the standardized cleaning agents can be used. In the current , edition the films, are cleansed only manually with the result that the method is not suitable for interlaboratory testing. Evaluate ease of removability in accordance with Tes: Methods D 3450 or D 4828. 10.2.3 Resistance to Household Chemicals--An impor tant property of interior coatings is the ability to resist spotting, softening or removal when subjected to household chemicals or strong cleaners. Determine resistance to these chemicals in accordance with Test Method D 1308. li-ins. I AS1M fl 10.3 Exterior Coalings: . .vi 10.3.1 Blister Resistance--Blister resistance is the ability 1 of a dry film on wood to resist the formation of blisters'' caused by water from the wood substrate. In practice water., can come from either the interior of a home or fron structural defects that permit entry of exterior water behind' the wood. Moisture blister resistance can be qualitatively evaluated in a laboratory test. Determine resistance to moisture blistering in accordance with Practice D 4585. 10.3.2 Exposure Resistance--Ifthe coating is intended for exterior use, evaluation of the resistance to weathering maj be required. In conducting exterior exposures follow Practice D 1006 for wood substrates or Test Method D 1014 for steel. 10.3.2.1 In establishing exterior performance on wood, use the panels described iiTSpecification D 358. 10.3.2.2 Degree of Chalking--Determine the rating using Methods D 659 or D 4214. 10.3.2.3 Degree of Checking--Determine the rating using Test Method D 660. 10.3.2.4 Degree ofCracking--Determine the rating using Test Method D 661. 10.3.2.5 Degree of Erosion--Determine the rating using- Test Method D 662. 10.3.2.6 Degree of Flaking--Determine the rating using Test Method D 772. 10.3.3 Mildew Resistance--Virtually all exterior paints are subject to microbiological discoloration on the surface with time. This is especially true in warm, moist climates. Determine mildew resistance in accordance with Practice D 3456. 10.3.4 Fume Resistance--Some paints exhibit a change in appearance (usually color) when exposed to air containing certain sulfur compounds, notably hydrogen sulfide and 970 A i DUP050298150 D 5146 ntn'Jl it7*3 Boh Of't jr.f lioxide. This type of atmosphere may be present near rial or other polluted areas and can cause paint to <or darken in as little time as overnight. There are no or Federal test methods for evaluating this color I, but one procedure used by the industry is as follows: |:4.1 Apply a sufficient number of coats of the paint to kss plates to hide the surface completely, allow to dry and expose one in a moist atmosphere of hydrogen I for 18 h. Compare the color with the unexposed plate, itposed plate should be practically no darker than the |osed one. The color difference should not exceed that eh plates that have been coated with a paint made with dioxide pigment, lead-free zinc oxide, raw or linseed oil, and sufficient cobalt added for drying, nilarly treated. jjfhating Analysis jf! Coating Analysis--If a specification requires certain jgiaterials or certain components in a given amount then Sis is needed to determine whether the specified com- hts are present and in what. amounts. Analysis is arily a measure of uniformity and does not necessarily |ish quality that can also be greatly affected by manu ring techniques. No single schematic analysis is compreve enough to cover the wide variety of paint composi- f Select test procedures from Methods D 215 and other methods that are pertinent to the components of Bnt-bome coatings. |!2 Volatile Content--The per cent of volatile matter is a jgure ofthe amount of a film lost as it dries. This quantity { necessarily indicative of the quality of the coating. It is however, for determining the similarity of two |es. The referenced method covers the determination of blatile content of solvent- and water-reducible coatings. Quantity determined subtracted from 100 % gives the |piatile content of the coating. Determine the volatile ent in accordance with Test Method D 2369. Of, [s3 Nonvolatile Content (Volume Percent)--The nonvolay' : content by volume is a useful figure in calculating a* age or spreading capacity per gallon (or litre) at a d |fied dry-film thickness. Determine nonvolatile content line percent in accordance with Test Method D 2697. 11.4 Water Content--If too much water is incorporated in a solvent-reducible coating it may retard the drying at high relative humidities. The amount of water in a coating is required in the calculation of the volatile organic content (VOC) of coatings. One referenced method covers the determination of water in paint and related materials by distilling with a volatile solvent. The newer method utilizes the Karl Fischer reaction. Determine water in accordance with Test Methods D 1208 or D 4017. 11.5 Pigment Content--Pigment provides the hiding and color and influences many other properties of a coating. The referenced method describes the procedure for the quantita tive separation of the vehicle from the pigment in solventreducible coatings. It is used to measure the weight percent pigment in the paint. Determine the percent pigment con tent in accordance with Test Method D 2371. 11.6 Pigment Analysis--The analysis of pigment may be required if the product is covered by a specification or upon agreement between the purchaser and seller. Analyze the pigment in accordance with selected test procedures from Methods D 215 and other appropriate ASTM methods. 11.7 Nonvolatile Vehicle Content--The nonvolatile ve hicle is the film-forming portion of a coating excluding the pigment. Water, volatile thinner, and pigment are deter mined and their sum subtracted from 100 % to give the binder content in accordance with Methods D215. The vehicle may be separated for further analysis. 11.8 Separation of Vehicle--The recommended proce dure describes this separation for certain solvent-borne coatings. If desired or required, separate the vehicle in accordance with Method D 2372. 11.9 Identification of Nonvolatile Vehicle--The type of. binder used in a coating has a great influence on its properties. The referenced method covers the qualitative characterization or identification by infra-red spectroscopy of separated nonvolatile vehicle. It is useful in detecting uniformity, batch to batch, and the presence of adulterants. Identify the nonvolatile vehicle in accordance with Method D2621. The composition of this vehicle can be further broken down into the types of oils present. If desired determine the identity of oils in accordance with Method D 2245. The American Society lor Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of Irte validity ot any such patent rights, and the risk ci inlringament ot such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every live years and Sgs it not revised, either reappreved or withdrawn. Yovr comments are invited either for revision ot this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ot the responsible Ig^ technical committee, which you may attend, tf you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ti' :e s. n 1-4 971 DUP050298151 0 5150 tion was found to be 0.5 rating units with 36 df. Based on these values the following criterion should be used for judging the acceptability of results at the 95 % confidence level: 10.1.1 Reproducibility--Two single results obtained by operators in different laboratories should be considered suspect if they differ by more than 1.5 rating units. 11. Keywords 11.1 architectural paints and coatings; hiding po- opacity; roller application of paints APPENDIX Nonmandatory Information XI. MANUFACTURER'S DESCRIPTION AND SPECIFICATIONS FOR THE PRACTICAL OPACITY CHARTS USED IN DEVELOPING THIS TEST METHOD5 XI.I Description and Specifications are as follows; XI.1.1 Overall Size--24 by 37Vt in. (610 by 953 mm), XL 1.2 Test Area--Size 24 by 36 in. (610 by 914 mm), 6 ft2 (5575 cm2), XL 1.3 Design--Alternate stripes of white and neutral grey, Xl.1.4 Stripe Dimensions--1J%2 by 36 in. (36 by 914 mm); XL 1.5 Stripe Numbers--The stripes are numbered 1 through 6 in order of increasing contrast, the numbers being printed on the two 24-in. borders. These borders are 34-in. (19-nvm) wide and are not normally considered a part of the test area. " XL 1.6 Unnumbered Stripes--The unnumbered stripes shown ip Figure 1 are an integral part ofthe test area; Their purpose is to favor application uniformity on the numbered stripes by preempting the boundary locations that tend to be less uniformly coated than more centrally located areas. X1.1.7 Grey Stripe Reflectances5--The reflectance values of the numbered stripes are selected with the objective that their color differences with respect to the white surround'.will be in the geometric sequence: 2,4, 8,16,32, and 64 CIELAB units. The defining variable for the grey stripes is not the reflectance as such, but the ratio of the grey reflectance G to the white reflectance W. Table XI. 1 shows the relevant relationships and production tolerances. NBD' Xl.l--The term "reflectance" as used here refers to the luminous reflectance factor as defined in 4.2 of Method E 97, which ` may be expressed as a decimal fraction or as a percentage. The latter is numerically the same as the CIE Y-tristimulus value and is the scale reading on most if not all commercial colorimeters. TABLE X 1.1 Relevant Relationships and Production Tolerances : Stripe Number 1 2 3 4 5 6 Color Difference,* % 2 12.5 4 12.5 8 12.5 16 i 12.5 32 12.5 64 12.5 Ratio G/Ws 0.945 0.007 0.893 0.013 0.793 0.024 0.617 0.042 0.347 0.055 0.067 0.037 Reflectance G.CS 75.8 + 0.6 71.4 1.0 63.5 1.9 49.4 3.4 27.8 + 4.4 5.3 3.0 - "This is AE`,0, the color difference with respect to the white stripes, expressed in CIELAB units as defined-in 6.2 of Method D 2244. aG/W = (1 - AE'ab/107.7)3. This equation is derived from 6.2.1 of Method D 2244 and assumes that for neutral grey versus white, the values AE*a0 and AL` are sufficiently close to be considered equal for the purpose of this test method. Values shown here are with a white stripe reflectance IV of 80 X. These values will vary somewhat with IV, tolerances for the latter being 2 % Inter-batch and 40.5 %. intra-batch. The American Society for Testing and Materials takes no position respecting the validity ot any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement ot such rights, are entirely their own responsibility. ____ This standard is subject to revision atany time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration af a meeting of the responsible technical committee, which you may attend, if you feet that your comments have not received a fair hearing you should make your views known to Me ASTM Committee on Standards, 1916 Race SI, Philadelphia, PA 19103. "; 1$; 218341-',' 9 74 DUP050298152 Designation: D 5161 - 91 Standard Guide for Specifying Inspection Requirements for Coating and Lining Work (Metal Substrates)1 This standard is issued under the fixed designation D 5161; the number immediately following the designation indicates the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon 0) indicates an editorial change since the last revision or reapproval. Scope SSPC-Visl-89 Visual Standard for Abrasive Blast Cleaned rs J&'l l This guide is intended to aid the coating specification Steel*5 ifiter in selecting and specifying the appropriate inspection Suirements. It indicates the inspection requirements that gy be employed for each of four service environments |luding mild, moderate, severe, and immersion (see Table 3. Terminology 3.1 Service Environments Terms are as follows: 3.1.1 mild service--indoor or protected outdoor areas not subject to rain,- dew or corrosive elements, or both. 11.2 In order to aid the user in determining when to specify Jppection requirements, a relationship between the consejHjsnce of failure and the suggested level of inspection is Hmonstrated (see Fig. 1). Bl ,3 It is not the intent ofthis guide to address the selection ^protective coating systems, to specify surface preparation 3.1.2 moderate service--areas subject to weather away from coastal or corrosive industrial environments, or both. 3.1.3 severe service--corrosive/erosive environments in cluding coastal salt laden atmosphere, industrial atmosphere, and high intensity sunlight. 3.1..4 immersion service--wetted surfaces of tanks, con tainers, pits, etc and surfaces that are normally wet with Ip application requirements, or to be a referenced docu- condensation or exposed to other corrosive environments. Rent in a specification. 4. Significance and Use Referenced Documents r-| 2.1 ASTM Standards: D,1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Metal Base2 D 1400 Test Method for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 ' D3276 Guide for Painting Inspectors (Metal Substrates)2 D4285 Test Method for Indicating Oil or Water in Compressed Air2 D 44 n Practice for Measurement of Wet Film Thickness by Notch Gages2 D4417 Test Method for Field Measurement of Surface Profile of Blast Cleaned Steel2 E 337 Test Method for Measuring Humidity with a Psychrometer (the Measurement of Wet and Dry-Bulb Temperatures)3 2.2 NACE Standard: T6A-37 Recommended Practice for Discontinuity, (Holi day Testing of Protective Coating)4 2.3 SSPC Standard: * This guide is under the jurisdiction or ASTM Committee D-33 on Protective gating and Lining Work for Power Generation Facilities and is the direct isponsibility of Subcommittee D33.04 ou Inspection. Current edition approved Aug. 15. 1991. Published October 1991. 2 Annual Book ofASTM Standards, Vol 06.01. ' A ivutal Book ofASTM Standards, Vol II .03. -4 Available from National Association of Corrosion Engineers, P.O. Box 118340. Houston, TX 77218. 4.1 The requirements for inspection should be addressed in all protective coating and lining work specifications. 4.2 This guide may be used by specification writers when selecting and establishing the inspection requirements for coating and lining specifications. 4.3 The instructions for using this guide are as follows: 4.3.1 Identify the service environment for the coating or linirig system being Specified. Read down the column under the appropriate service environment in Table I. Suggested levels of inspection listed on the left are identified with x's. 5. Inspection Requirements 5.1 Pre-Surface Preparation: 5.1.1 Contaminants--Visually verify that oil and grease are removed from the surface prior to surface preparation operations (See Guide D 3276). 5.1.2 Surface Anomalies--Visually verify that welds and sharp or jagged edges have been suitably prepared for the coating system being used (see Guide D 3276). 5.2 Surface Preparation: 5.2.1 Air Supply--Verify that air supply is clean and dry (see Test Method D 4285). 5.2.2 Abrasives--Verify cleanliness and proper size and type to achieve specified profile. 5.2.3 Ambient Conditions--Verify that air temperature, humidity, surface temperature, and due point spread are appropriate (see Test Method E 337). 5.2.4 Surface Anomalies--Identify any burrs, slivers, scabs, and Weld spatter visible after blasting. 5 Available from Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, PA 15213. 975 i ( DUP05 0298153 D 5161 TABLE 1 Inspection Requirements SERVICE ENVIRONMENT Sucaesied Inspection Requirements Service Environments Mild Moderate Severe Immersion {.MILO) {MODERATE) (SEVERE) (IMMERSION) Pre-Surface Preparation: Visual for contaminants X X X X SAFETY/flEGUUvrcAy VIOLATION Visual for surface XX anomalies Surface Preparation: Air supply for contaminants Abrasives for type and XX XX EFGH( FHG G DEGRADATION cleanliness Ambient conditions and XX . dew point Surface anomalies XX Degree of cleanliness X X X X 1PLANTOR EQUIPMENT DOWN TIME Profile X XX Visual final for X- X contamination Coating Application: Materials - X X X- INCREASED REPAIR COST Mixing XX Equipment XXX Air supply for XXX contaminants Ambient conditions and X , X SUGGESTED LEVEt OF INSPECTION dew posit Wet film thickness XX LOW MEDIUM HIGH Intercoat parameters Appearance between coats Dry film thickness between coats Final Acceptance: Appearance Visual runs and sags Visual holidays and X X X' X X X X' 8 XX ;/ XX XX , NIJ' --;This figure Is' provided, as a visual aid to represent graphically; ihe ,* general relationship betweenIhe consequenceof failure and the suggested levelC Inspection.- The slope and configuration of the curve will vary due bo tiie many * factors affecting the consequence of failure, however, the suggested level of inspection should increase when the service environment is more severe. FIG. 1 Relationship Between the Consequence of Failure and the Suggested Level of Inspection pinholes Dry film thickness Holiday tests Repairs Final cure XXX 5.3.8 Appearance--Visually inspect each coat for defers ^ X and uniform appearance (see Guide D 3276). X X X X 5.3.9 Dry Film Thickness--Verify that the dry film thick ness is within the specified range after each coat (see Test Methods D 1186 and D 1400). 5.2.5 Surface Cleanliness--Verily degree of surface clean 5.4 Final Acceptance: liness (see SSPC-Visl-89). 5.-2.6 Profile--Verify profile is within specified tolerance using appropriate instruments (see Test Method D 4417). 5.2.7 Surface Contamination--Verify-that-all visible .Sur face contaminants including oil, grease, dust, etc have been removed;' ., 5,3 Coating Application: > ,. 5.3.1 Materials--Verify that the coating materials and thinners are as specified, properly labeled and stored, and are within their shelf life. 5.3.2 Mixing--Verify that the coating materials are mixed in accordance with the manufacturer's instructions. 5.3.3 Equipment--Verify that proper application equip 5.4.1- Appearance--V. isualfy inspect the surface for defec.s and uniform appearance (see Guide D 3276); 5.4.2 Dry Film Thicfcness-r-Verify that the total coatino system's dry film thickness is within the specified range (see Test Methods D 1186 and D 1400). 5.4.3 Holiday Test--Verify that the surface meets tin specified holiday/pinhole criteria (see NACE T6A-37). 5.4.4 Repairs--Verify that all identified repairs have bee n properly made. Repeat inspection requirements and testing ; as appropriate. 5.4.5 Final Cure--Verify that the coating is cured in accordance with the' specified requirements of Guide D 3276. ment is being utilized. 6. Precautions and Limits 5.3.4 Air Supply--Verify that ajr supply is clean and dry (see Test Method D 4285). 5.3.5 Ambient Conditions--Verify that air temperature, humidity, surface temperature, and dew point spread are appropriate (see Test Method E 337). 5.3.6 Wet Film Thickness--Verify that the applicator is checking wet film thickness during, the application process when required (see Practice D 4414). 5.3.7 Intercoat Parameters--Verify that parameters 6.1 Specialty lining systems such as reinforced laminates may have additional inspection requirements to address hardness, strength, etc that are not addressed by this guide 6.2 The quality of a project cannot be guaranteed b merely specifying inspection requirements, however, whe.i the recommended inspections are properly implemented and documented, failures are minimized or eliminated. 7. Keywords during recoat are observed and that no surface contaminants 7.1 coating, inspection, specifications; consequence ' are present. failure; level of inspection; linings 976 I H o i. t; 'L \| A ! ? if. gIIf t? DUP0502981 54 # D 5181 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted' in connection with any item mentioned in this standard. Users of this standard are expressly advised that defer/wnaf/on of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision ar any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapprovedor withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 977 DUP0502981 55 4 Designation: D 5162 - 91 Standard Practice for Discontinuity (Holiday) Testing of Nonconductive Protective Coating on Metallic Substrates1 2 This standard is issued under the fixed designation D 5162; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or ieapprcival. 1. Scope 1.1 This practice covers procedures for determining discontinuities using two types of test equipment: i. 1.1 Test Method A--Low Voltage Wet Sponge, and 1.1.2 Test Method B--High Voltage Spark Testers. 1.2 This practice addresses metallic substrates. For con crete surfaces, refer to Practice D 4787.3 1:3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D4787 Practice for Continuity Verification of Liquid or Sheet Linings Applied to Concrete Substrates3 3. Terminology 3.1 Description of Terms Specific to This Standard: 3.1.1 discontinuity, as used in this standard--a void, crack, thin spot, foreign inclusion, or contamination in the coating film that significantly lowers the dielectric strength of the coating film. May also be identified as a holiday or pinhole. 3.1.2 holiday, as used in this standard--a term that identifies a discontinuity. 3.1.3 holiday detector, as used in this standard--a device that locates discontinuities in a nonconductive coating film applied to a conductive surface. 3.1.4 pinhole, as used in this standard--a film defect characterized by small porelike flaws in the coating which, when extended entirely through the film, will appear as a discontinuity. A pinhole in the finish coat may not appear as a discontinuity. 4. Significance and Use 4.1 A coating is applied to a metallic substrate to prevent corrosion, reduce abrasion or reduce product contamination, or both. The degree of coating continuity required is dictated by service conditions. Discontinuities in a coating are frequently very minute and not readily visible. This practice provides a procedure for electrical detection of minute 1 This practice is under the jurisdiction of ASTM Committee D~33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility of Subcommittee D33.04 on Inspection. Current edition approved Sept. 23, 1991. Published November 1991. 2 Annual Book ofASTM Standards, Vol 06.01. discontinuities in nonconductive coating systems. 4.2 Electrical testing to determine the presence aiul number ofdiscontinuities in a coating film is performed on j nonconductive coating applied to a conductive surface. TLe allowable number of discontinuities should be determined ' prior to conducting this test since the acceptable quantiiy of ^ discontinuities will vary depending on coating film thickness, j design, and service conditions. | 4.3 The loft voltage wet sponge test equipment is genet- .1 ally used for determining the existence of discontinuities in I Jcoating films having a total thickness of 20 mils (0.5 mm) or t less. High voltage spark test equipment is generally used for determining the existences of discontinuities in coating films Jg having a total thickness of greater than 20 mils (0.5 mm) * 4.4 Coatings that are applied at a thickness of less than 20 j mils (0.5 mm) may be susceptible to damage if tested with i high voltage spark testing equipment. Consult the coatine 1 manufacturer for proper test equipment and inspectur voltages. ^ 4.5 To prevent damage to a coating film when using higjjrf) voltage test instrumentation, total film thickness and dielecrifS trie strength in a coating system shall be considered m,fl| selecting the appropriate voltage for detection af.J discontinuities. Atmospheric conditions shall also be consid- M ered since the voltage required for the spark to gap a given % distance in air varies with the conductivity of the air at the * time the test is conducted. Suggested starting voltages are j provided in Table 1. 4.6 The coating manufacturer shall be consulted to obtain |j the following information, which would affect the accuiacy j of this test to determinediscontinuities: I 4.6. i Establish the length of time required to adequately | dry or cure the applied coating film prior to testing. Solvni-, 1 retained in an uncured coating film may form an electrically $ conductive path through the film to the substrate. f 4.6.2 Determine whether the coating contains electrically | rtl TABLE 1 Suggested Voltages for High Voltage Spark Testing Total Dry Film Thickness mils mm 8-12 13-16 19-30 31-40 41-60 61-80 81-100 101-125 126-160 161-200 201-250 0.20-0.31 0.32-0.46 0.47-0.77 0.78-1.03 1.04-1.54 1.55-2.04 2.05-2.55 2.56-3.19 3.20-4.07 4.08-5.09 5.10-6.35 1 500 2 000 2 500 4 000 5 000 7 500 10 000 12 000 15 000 20 000 25 000 o. riithl DUP05Q298156 # D 5162 nductive fillers or pigments that may affect the normal |ectric properties. *7 This practice is intended for use with new coatings. It also be applicable for coatings previously placed in vice. However, considerations must be given to potential nges in the electrical properties of the coating due to |ervice exposure. Test Methods METHOD A--LOW VOLTAGE WET SPONGE TESTING Apparatus e aiul jfri.I Low Voltage Holiday Detector--an electronic de- ft nil a 41 powered by a self-contained battery with voltages e. The jjjging from 5 to 90 V dc' depending on the equipment miny nufacturer's circuit design. It is used to locate itity-'ajn Continuities in a nonconductive coating applied to a :kncw, nductive substrate. Operation includes the use of an (fen-cel! sponge electrode wetted with a solution for ex gener-j iling'the coating surface, a ground connection, and an sties in ; dible or visual indicator, or both, for signaling a point of lm) or I gting discontinuity. sod for i 3.1.2 Low Voltage Wet Sponge Tester--a sensitivity de- S films| with the operating voltage being of little importance vn) ler than being part of the particular electronic circuit tar. 201 sign. . d 1.3 Wet Sponge Type Instrument--a number of com- omini-i Ircially available, industry-accepted, instruments are avail- union' jje. The following electronic principle describes two types jdevices generally used; others may be available but are not ig bigtiS |cribed in this practice. dielec- '1 5.1.3.1 Lightweight, Self-Contained, Portable Devices-- red (!!_ jfsed on the electrical principle of an electromagnetic )il llf` gnsuive relay or a solid-state electronic relay circuit that V lSlll-' jergizes an audible or visual indicator when a coating i givelfl continuity is detected. Generally this equipment is ca- at mu Ifele of being recalibrated in the field by the user. ;es aie1 15.1.3.2 Lightweight, Self-Contained, Portable Devices-- jo based on the principle of an electronic relaxation obi r.ip jjpllator circuit that reacts significantly to the abrupt drop curacy S electrical resistance between the high dielectric value of gfe coating film and the conductive substrate at the point of luatelyf gating film discontinuity. This results in a rise in oscillator >lvenii fluency as well as in the audible signal from the device, ;ricaity| fsnerally, this equipment is incapable of being recalibrated |the field by the user. TirallyJ Procedure isting [5,2.1 Sufficient drying or curing of the coating shall be lowed prior to conducting a test. The length of time stion, V fi Suited shall be obtained from the coating manufacturer. llvents retained in the coating film could produce erro- Ipus indicators. 15.2.2 The surface shall be clean, dry, and free, of oil, dirt lid other contaminates. Measure the film thickness of the gating with a nondestructive dry film thickness gage. If the |ating film exceeds 20 mils (0.5 mm), use the. procedures high voltage spark testing described in Test Method B, fgh Voltage Spark Testing. |5.2.3 Test the instrument for sensitivity in accordance |th 5.3. 5.2.4 Attach the ground wire from the instrument ground output terminal to the metallic substrate and ensure positive electrical contact. 5.2.5 Attach the exploring sponge lead to the other output terminal. 5.2.6 Wet the sponge with a solution consisting of tap water and a low sudsing wetting agent, combined at a ratio of not more than xh fluid oz of wetting agent to 1 gal water. An example of a low sudsing wetting agent is one used in photographic development. The sponge shall be wetted sufficiently to barely avoid dripping of the solution while the sponge is moved over the coating. The wetting agent residue must be removed prior to executing repairs. n 5.2.7 Sodium chloride (salt) shall not be added to the wetting solution because of the potential erroneous indica tions of discontinuities. The salt, after drying on the coated surface, may form a continuous path of conductivity. It will also interfere with intercoat adhesion of additional coats. 5.2.8 Contact a bare spot on the conductive substrate with the wetted sponge to verify that the instrument is properly grounded. This procedure shall be repeated periodically during the test. 5.2.9 Move the sponge over the surface of the coating at a moderate rate approximately I ft/s (0.3 m/s), using a double pass over each area. Apply sufficient pressure to maintain a wet surface. Ifa discontinuity is detected, turn the sponge on end to determine the exact location of the discontinuity. 5.2.10 Discontinuities that require repair shall be identi fied with a marker that is compatible with the repair coating or one that is easily removed. 5.2.11 To prevent telegraphing (current traveling through a moisture path to a discontinuity, giving an erroneous indication), take care to ensure that the solution is wiped dry from a previously detected discontinuity before continuing the test. 5.2.12 The wetting agent must be completely removed by rinsing the holiday area prior to repair. 5.2.13 Wet sponge holiday detection is not recommended between coats of a multicoat system. However; when a test is conducted between coats of a multicoat system, a wetting ageht shall not be used and all residue left by the test water must be completely removed prior to applying additional coats. 5.3. Verifying Operation of Equipment 5.3.1 The instrument shall be tested for sensitivity prior to initial use and periodically thereafter, in accordance with the equipment manufacturer's instructions. 5.3.2 Test the battery for proper voltage output. Refer to the manufacturer's instructions. 5.3.3 Switch the instrument to the "on position," if applicable. 5.3.4 Wet the sponge with a wetting solution consisting of tap water and a wetting agent (see 5.2.6). 5.3.5 Connect the ground cable to the instrument ground output terminal. 5.3.6 Touch the ground cable alligator clip to the wetted sponge. The instrument signal should actuate in accordance with the instrument manufacturer's instructions. 5.3.7 If the instrument should fail to signal, it shall be considered defective. 979 DUP0502981 57 D 5162 5.4 Verifying Instrument Calibration 5.4.1 Verify instrument calibration in accordance with the manufacturer's latest published instructions. If out of cali bration, the instrument shall be calibrated in accordance with the instrument manufacturer's latest published instruc tions, or returned for calibration. TEST METHOD B--HIGH VOLTAGE SPARK TESTING 5.5 Apparatus 5.5.1 High Voltage Detector (in excess of 800 V)--An electronic device used to locate discontinuities in a nonconductive protective coating applied to a conductive substrate. It consists of an electrical energy source, an exploring electrode, and a ground wire connection from the indicator signaling current flow through a coating filih discontinuity to'the substrate. The defector shall be equipped with a visual1 or audible indicator, or both. 5.5.2 Exploring Electrode, shall be of the type capable of maintaining continuous contact with the surface being inspected, such as bolts, raised areas, etc. It shall be kept clean and free of coating material. 5.5.3 High Voltage Electrical Detector, can be identified as either a pulse or direct current type. A pulse type detector discharges a cycling, high voltage pulse, while a direct current type discharges continuous voltage. 5.6 Procedure 5.6.1 Sufficient drying or curing of the coating shall be allowed prior to conducting a holiday test, The length of time required shall be obtained from the coating manufac turer. Solvents retained in the coating film could produce erroneous results, as well as a fire hazard. 5.6.2 The surface shall be clean, dry, and free of oil, dirt and other contaminates. Measure thickness of, the coating with a nondestructive dry film thickness gage. If the coating film is less than 20 mils (0.5 mm), consider using procedures for low voltage testing (see Test Method A, Low Voltage Wet Sponge Testing). Although the high voltage spark tester is suitable for determining discontinuities in coating films of less than 20 mils (0.5 mm), it is recommended that the coating manufacturer be consulted before using this test. Certain coatings may be damaged if tested with this equip ment. 5.6.3 Verify test instrument operation in accordance with 5.7. 5.6.4 Adjust the test instrument to the proper voltage for the coating thickness being tested. In selecting the inspection voltage, it is important to provide sufficient voltage to break the air gap that exists at the holiday. The air gap will vary depending on the total applied film thickness. The voltage required to break a given air gap may also vary due to atmospheric conditions such as relative humidity. Ensure that the voltage is high enough to break the air gap equivalent to the highest coating film thickness by separating the exploring electrode from the bare metal substrate using a nonconductive spacer equal to the maximum coating thick ness. The voltage is set high enough to conduct the holiday test only if the spark will jump the gap formed by the spacer. Excessive voltage may produce a holiday in the coating film. The maximum voltage for the applied coating shall be obtained from the coating manufacturer. Table 1 contains suggested voltages that can be used as guides. 5.6.5 Attach ground wire from the instrument ground output terminal to the metal substrate and ensure positive electrical contact. 5.6.6 Make contact with the exploring electrode on the conductive substrate to verify that the instrument is properly grounded. This test shall be conducted periodically during' the test. The spacer test described in 5.6.4 shall also be repeated ifsignificant atmospheric changes take place during testing. 5.6.7 Move the exploring electrode over the surface of tlv dry coating at a rate ofapproximately 1 ft/s (0.3 m/s) using a single pass. Moisture on the coating surface may cause erroneous indications. If moisture exists, remove or allow dry before conducting test. 5.6.8 Discontinuities that require repair shall be identified with a marker that is compatible with the repair coating or one that is easily removed. 5.7 Verifying Operation of Equipment 5.7.1 Test the energy source (battery) for proper voltage output. Refer to the manufacturer's instructions. 5.7.2 Connect the exploring electrode and grounding cable to the terminals of the detectors. 5.7.3 Switch the instrument to the "on" position. 5.7.4 Touch the exploring electrode to the ground cable alligator clip. The instrument signal should actuate in accordance with the instrument manufacturer's operating instructions. 5.7.5 If the instrument fails to signal, it shall be considered defective. 5.8 Verifying Instrument Calibration 5.8.1 Verify instrument calibration in accordance with the manufacturer's latest published instructions. If out of cali bration, the instrument shall be calibrated in accordance with the instrument manufacturer's latest published instruc tions, or returned for calibration. 5.8.2 Perform field checking of the test voltage with the electrode placed, against the surface of the lining since tin. exploring electrode voltage may be reduced by the slight current flow of the lining. 5.8.3 If required, compare measured voltage with the selected test voltage. Depending on the type of tester, adjust the selected voltage 5 %. 6. Testing of Repaired Area 6.1 Sufficient drying or curing of the repair coating shall be allowed prior to retesting. The length of time required shall be obtained from the coating manufacturer. 6.2 Conduct the test following the procedures as previ ously outlined in this practice for the test instrument selected. 6.3 Retest only those areas that have been repaired, unless otherwise specified. 7. Keywords 7.1 discontinuity; holiday; holiday detectors; spark testei- 980 DUP050298158 # D 5162 The American Society for Testing and Materials takes no position respecting the validity of anypatent rights asserted in connection with any Item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement oI such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnor revised, eitherreapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050298159 Designation: D 5163 - 91 Standard Guide for Establishing Procedures to Monitor the Performance of Safety Related Coatings in an Operating Nuclear Power Plant1 This standard is issued under the fixed designation D 5163 ; the number immediately following the-designation indicates the year of original adoption nr, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. .hi " Hid 1. Scope 1.1 This guide extvers procedures for establishing a pro gram to monitor Service Level I coating systems in operating nuclear power plants. Monitoring is an on going process of evaluating the condition of the in-service coating systems. 1.2 It is the intent of this guide to provide a recommended basis for establishing a coatings monitoring program, not to mandate a singular basis for all programs. Variations or simplifications of the program described in this guide may be appropriate for each operating nuclear power plant de pending on their licensing commitments. Similar guidelines may be applicable for Service Level II and other areas outside containment. 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 610 Test Methods for Evaluating Degree of Rusting on Painted Steel Surfaces2 D 714 Test Method for Evaluating Degree of Blistering of Paints2 D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D3359 Test Methods for Measuring Adhesion by Tape Test2 D4121 Practice for Photographic Documentation of Coating and Lining Failures and Defects2 D4537 Guide for Establishing Procedures to Qualify and Certify Inspection Personnel for Coating Work in Nu clear Facilities2 D4541 Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers2 F 1130 Practice for Inspecting the Coating System of a Ship's Topside and Superstructure3 F 1131 Practice for Inspecting the Coating System of a ' Ship's Tanks and Voids3 F 1132 Practice for Inspecting the Coating System of a Ship's Decks and Deck Machinery3 :F 1133 Practice for Inspecting the Coatipg Syste.m.. uofi . --: Ship's Underwater Hull and Boottop D"uring 'finds Drydocking3 2.2 ANSI Standard: F N45.2.6--Qualification of Inspection, Examination, and Testing Personnel for Nuclear Power Plants4 2.3 SSPC Standard: SSPC-PA2--Measurement of Dry Paint Thickness With Magnetic ages5 2.4 NACE Standard: RP0188-88--Standard Practice Discontinuity (Holiday) Testing of Protective Coatings6 3. Significance and Use 3.1 Establishment of an in-service coatings monitoring program permits planning and prioritization of coatings maintenance work as needed to maintain coat integrity and performance in nuclear Service Level I coating systems, additional information on nuclear maintenance coa work, refer to ASTM Manual on Maintenance CoatingsifbrJ Nuclear Power Plants.7 3.2 A coatings monitoring program enables early identifi cation and detection of potential problems in coating sys tems. Some Service Level I coating systems may be known if advance to be suspect, deficient, or unqualified. Monitoi coating performance will assist in developing follow-up procedures to resolve any significant deficiency relative to coating work. 3.3 Degraded coatings may generate debris under design basis accident conditions that could adversely affect the performance of the post-accident saf:ety systems. A coatings .. Cf -o64.l..if, monitoring program may be required1 to fulfill safety analysis 1 jtplacej^ report commitments for Service Levveel I coating work in a I If 6.2.3| nuclear power plant facility. 644 4. Responsibility rk PJ 4.1 The owner/operator shall identify the department or group within the organization to be responsible for estab lishing the applicable requirements for activities or proce: dures covered by this guide and shall document the scope of their responsibility. Owner/operator delegation of this re sponsibility to other outside qualified organizations is per- 1 This guide is under the jurisdiction of ASTM Committee D-33 on Protective Coating and Lining Work for Power Generation Facilities and is the direct responsibility ofSubcommittee D33.04 on Inspection. Current edition approved Oct. 3, 1991. Published December 1991. 2 Annual Book ofASTM Standards, Vol 06.01. ? Annual Book ofASTM Standards, Vol 01.07. 4 Available from American National Standards Institute, JI W. 42nd Street, 13th Floor, New York, NY 10036. 5 Available from Steel Structures Painting Council, 4400 Fifth Ave., Pittsburgh, PA 15213. 6 Available from National Association of Corrosion Engineers, P. O. Box 218340, Houston, TX 77218. 7 Available from ASTM Headquarters, 1916 Race St., Philadelphia, PA 19103. 982 DU P05 02 98160 D 5163 rstem of j ) Dunns itted and shall be documented. |4.2 It is the responsibility of the owner/operator or his isignee performing these activities to specify the detailed iethods and procedures For meeting the applicable require ments of this guide. j4.3 The owner/operator or his designee shall assign a ordinator to be responsible for supervising coating inspec- j|n activities, data collection and documentation, and for uring that inspection personnel are adequately trained id qualified. 4.4 The owner/operator shall assign responsibility for !aluating the results of inspection activities carried out *fider the coatings performance monitoring program. 1. jjS. Frequency ation, unit > 5.1 Frequency of in-service coating inspection monitoring i I. ill be determined by the owner/operator. In operating 1 femclear power plants certain monitoring activities may be :ness Vi ith t Restricted to major maintenance outages or refueling outages. ' 'f,lj is a good practice to perform inspections during each ^ ^rcfiieling outage or during other major maintenance outages (Holiday)| ||s needed. t Records and Past History % 6.1 Coating performance will depend on the operating nonitonnn i (conditions experienced by the coating systems. Records of f coatiiy, Jiese WcoUnUd1itUioUnIUs osuhaanll Ubelr UobUtKaUinIHe,Ud 1foU1r ke.aaciohi Ko>p;ve,>rLat<inM6g< ujn.nitl. :egrity and^: *1 hese may include, but not be limited to, ambient condistems. 1 or* 'jtions, temperatures, humidity, immersion, splash and :e coaling sspillage, chemical exposures, radiation exposures, previous ratings for, t ^decontamination procedures, abrasioh and physical abuse, J (Find start-up/shutdown frequency. Any change in service lyidentifi-^ ^criteria or modifications of the physical design must be taring sylfl Mentified and dated. known in iSJjfcii 6.2 The last two performance monitoring reports perdonitoringlSKpining to the coating systems shall be reviewed prior to the follow-up,umitoring process. Other past coatings history data to be relative to (#j[r;viewed may include; 6.2.1 Copies of coating specifications, manufacturer's der desigiUiKpproduct data sheets, and application procedures for in-place affect 1 , IE itings. \ coatin ,ii djjjt 6.2.2 Quality control documentation for the existing inty analyua-'p'ace coating systems and their application, work in a*,6.2.3 Copies of previous inspection or monitoring reports. 6.2.4 Documentation pertaining to any maintenance work performed on existing coating systems. rtment tsta Premonitoring Procedure for estal 7.1 Prior to conducting an inspection of the coating or proci ystems, the responsible organization shall ensure that the e scope o: fiecessary services and equipment required for inspection are if this r& provided. Factors that must be considered while planning the ns is pef- Inspection activities include, but are not limited to, lighting, Jccess to coated surfaces, cleaning surfaces of any deposit or build up, ventilation and, where necessary, special under water inspection requirements. 7.2 Station access procedures for Service Level I coating |ystems monitoring shall be followed. While access proce dures may vary from plant to plant, specific station access procedures may include: 7.2.1 Security clearance for protected, radiation con- trolled, and vital areas, and escorted or unescorted clearance as required, 7.2.2 Radiological history including prior radiation expo sure for all personnel involved, 7.2.3 Health, physics classroom training in the use of radiation detection and monitoring devices and procedures for wearing anticontamination clothing, 7.2.4 A radiation wqrk permit based on health physics radiological survey of the work location, 7.2.5 Compliance with radiation work permit require ments and other special radiation controls unique to each work location, and 7.2.6 Issuance of dosimetry. " 7.3 The safety requirements of the facility owner/operator must be met when performing all inspection operations. 8. Personnel Requirements, Qualifications, and Training 8.1 The facility owner/operator shall specify the require ments and guidelines for qualification and training of inspection personnel involved in the program. However, inspectors and the coordinator shall be knowledgeable coat ings personnel meeting the requirements of ASTM Guide D4537 or ANSI N45.2.6. The coordinator shall, as a minimum, be a Level II Coatings Inspector. 8.2 The evaluator shall be a person knowledgeable and experienced in nuclear coatings work. 9. Inspection Plan 9.1 The owner/operator shall develop a plant specific inspection plan to accomplish the objectives of the moni toring program. A general visual inspection shall be con ducted on all readily accessible coated surfaces during a walk-through. After the walk-through, thorough visual in spections shall be carried out on previously desigfiated areas and on areas noted as deficient during the walk-through. A thorough visual inspection shall also be carried out on all coatings near sumps or screens associated with the Emer gency Core Cooling System (ECCSj. The inspection plan shall address the following based on specific owner/operator requirements: 9.1.1 A pre-inspection briefing to familiarize, all inspec tion personnel with objectives of the inspections, procedures to be followed, and precautions to be taken, 9.1.2 Monitoring team(s) assignments to specific areas for inspection(s), and 9.1.3 Location maps dividing the plant into identifiable areas for inspection activities to be issued to inspection teams. The maps shall also identify items/areas requiring special testing, if any. The locations of all defects and of all tests performed shall be recorded on the maps so that additional testing, recoating, and further monitoring may be performed. 9.2 During walk-through, visually examine coated sur faces for any visible defects, such as blistering, cracking, flaking/peeling, rusting, and physical damage. 9.2.1 Blistering--Compare any blistering found to the blistering pictorial standards of coatings defects (refer to Test Method D 714) and record size and frequency. If the blisters are larger than those on the comparison photographs, measure, record size and extent, and photograph. Report if blistered portions are intact. i %y r~ l. 983 DUP050298161 # D 5163 9.2.2 Cracking--Cracking can be limited to the one layer of coating or extend through to the substrate. Measure the length of the crack or if extensive cracking has occurred, measure the size of the area affected. Determine if the cracking is isolated or is part of a pattern. Record measure ments and describe crack depth and pattern on the inspec tion report. Photograph the area affected. 9.2.3 Flaking/Peeling/Delamination--Measure the ap proximate size of the peels and note the pattern formed. Carefully test to see if lifting can be easily achieved beyond the obvious peeled area. Note all observations on the inspection report and photograph the area affected. 9.2.4 Rusting--Compare with the pictorial standards of Test Method D 610 to determine the degree of rusting. Try to determine the source of rusting (that is, is it surface stain caused by rusting elsewhere, or is it a failure of the coating allowing the substrate to rust): Photograph the affected area and record observations on the inspection report. 9.2.5 If no defects are found, mark "Coating Intact, No Defects" on the inspection report. 9.2.6 If portions of the coating cannot be inspected, note the specific areas on the location map-inspection report, along with the reason why the inspection cannot be con ducted. 9.3 Written or photographic documentation, or both of coating inspection areas, failures, and defects shall be made and the process of documentation standardized by the facility owner/operator. Written documentation practice for inspection of coating system as given in Practices F 1130, F 3131, F1132, and F 1133 may be adopted as a guideline. Practice D4121 provides one method to obtain consistent, comparable close-up photographs. 9.4 For coating surfaces determined to be suspect, defec tive or deficient, one or more physical tests, such as dry film thickness (Test Methods D 1186 and SSPC-PA-2), adhesion (Test Methods D 3359 and D 4541), and continuity (NACERP0188-88), may be performed when directed by the eyaluator. Samples may be gathered, and the size and extent of defective patterns may be described. 9.5 Instruments and equipment needed for inspection may include, but not be limited to, flashlights, spotlights, marker pen, mirror, measuring tape, magnifier, binoculars, 35-mm camera with or without wide angle lens, and polyeth ylene zip lock sample bags.10 COATINGS PERFORMANCE MONITORING PROGRAM ImpecttaARepcn*: Turn *: _____ Urttlr 1 i SurveyDate____ Work Package m PAJtT GENERALVIS(ML INSPECTION SeeSurveyMipi: _________ Heat DLeosccariptiotinon/ GcncnlCQjtiticCsBdlbon Sal/ Uniat VPidheooto1/C e[/reascckriinbiec.cdornvd1it0iomnt1h/icuknnaeassii,sNfin9oIIrOy(: (nInucillundre.:stbmlisoteleriNngn. -- FIG. 1 Inspection Data Sheet MKC ELBE* 1*0* ARW/xpin*. seuthkttt Quttfnnt * .. tw SATX Toot nm -mTio'tO.i i r: 1 1 1 t ^Tm1--1--CAL. Mt/SVT HO. DATE------ I ITU. 10.Reporting and Documentation 10.1 Inspection reports for submittal to responsible eval uation personnel based on specific owner/operator require ments should be prepared by a qualified Level II or Level III Coatings Inspector and should include at least the following information; 10.1.1 A list and location of all areas evidencing deterio ration, 10.1.2 Prioritize the repair areas into areas that must be repaired during the same outage and areas where repair can be postponed to future outages, keeping the coating under surveillance in the interim period, 10.1.3 Inspection Data Sheets--A typical data sheet is given in Fig. l, and 10.1.4 Photographic Documentation--A typical location map for photographic identification is given in Fig. 2. The A3.. FaArsUACMOOtrf-Lee-BJ-APTZMPSZ5LA*T.aOK. *4 D. PIPING c. emeu Pl a t a FIG. 2 Photographic Documentation Location Map DUP050298162 0 5163 -n and direction of all photographs shall be recorded maps for comparison with past and future photoand to record existing conditions. Numbers 3-1 3-13 in Fig. 2 depict the location of the photogra- ;d the directions of the view. palliation The inspection report shall be evaluated by the ' sible evaluation personnel. The evaluator shall prea report that includes a summary of findings and mmendations for future surveillance or repair; this would include an analysis of the reasons or suspected reasons for failure. The repair work should be prioritized into major and minor defective areas. A recommended corrective plan of action must be provided for the major defective areas so that the plant can repair these areas, if appropriate, during the same outage. 12. Keywords 12.1 coatings monitoring program; coating performance; inspection; maintenance; nuclear power plant; safety related coatings; Service Level I; surveillance The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are exprass/y advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technicai committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision ofthis standard or for additional sfancferds and should be addressed to ASTM Headquarters. Your comments wilf receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 985 DUP050298163 (jjjjM Designation: D 5178 - 91 Standard Test Method for Mar Resistance of Organic Coatings1 |d th : feh m This standard is issued under the fixed designation D 517S; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval, superscript epsilon () indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the determination of the mar resistance on smooth, flat surfaces. Results are expressed in terms of force-to-mar films of organic coatings such as paint, varnish, and lacquer when applied to smooth, flat planar panel surfaces. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user of this standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D 609 Methods for Preparation of Steel Panels for Testing Paint, Varnish, Lacquer, and Related Products2 D823 Test Methods for Producing Films of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels2 D1005 Test Method for Measuring of Dry^Film Thickness of Organic Coatings Using Micrometers2 D 1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous Base2 D1400 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonconductive Coatings Ap plied to a Nonferrous Metal Base2 D269I Test Methods for Microscopical Measurement of Dry Film Thickness of Coatings on Wood Products2 3. Terminology '3.1 mar resistance--the ability of a coating to resist damage caused by light abrasion. As just defined, it is a resistance of the surface of the coating to permanent defor mation, resulting from the application ofa dynamic mechan ical force. 4. Summary of Test Method 4.1 The materials under test are applied at uniform thickness to flat panels of uniform surface texture. After drying/curing, the mar resistance is determined by pushing the panels beneath a rounded stylus or loop that is loaded in increasing amounts until the coating is marred. J This test method is under the jurisdiction of ASTM Committee D-l on Paints and Related Coatings and Materials and is the direct responsibility of Subcommittee D01.23 on Physical Properties of Applied Paint Films. Current edition approved Oct. 15, 1991. Published December 1991, 2 Annual Book ofASTM Siundards, Vol 06.01. 5. Significance and Use 5.1 In some situations, marring of coatings applied to substrates under typical use conditions is unacceptable. This test method has been found useful in differentiating ih,, degree of marring of coatings on substrates. It is most usefij in providing relative ratings for a series of coated panels exhibiting significant differences in marring. 6. Apparatus 6.1 Application Equipment, as described in Test Methods D 823. 6.2 Film-Thickness Measuring Apparatus, as described in Test Methods D 1005, D 1186, D 1400, or D 2691. 6.3 Balanced Beam Scrape Adhesion and Mar Test,r (Figs. 1 and 2),3 consisting of a balanced beam to which i>. secured a platform for supporting weights, and a rod at an angle of 45 that holds the scraping loop, a polished chromium plated steel rod hardened to Rockwell 56 to 58 The loop shall be a Via-in. (1.6-mm) diameter rod bent into a "U" shape with an outside radius of 0.128 0.002 in. (3.25 0.05 mm). These testers are adjustable to accommodate flat, metallic, and nonmetallic specimens to 0.5 in. (12 min) thick and 4 to 16 in. (100 to 400 mm) wide and long; the specimen should be at least xh in. (12 mm) wide. 7. Preparation of Specimens 7.1 Apply the materials under test to panels of the composition and surface condition on which it is desired to determine mar resistance of the coating. The panel material (7.1.1), surface preparation, thickness, and number of coats shall be specified or agreed upon between the seller and the purchaser. Apply coatings ancLair dry or bake under condi tions of humidity and temperature mutually agreeable to the seller and the purchaser. 7.1.1 The surface of the coating must be hard enough to resist damage by the scraping loop at a load agreed upon between the producer and the user. If no panel material specified, use 0.032-in. (0.8-mm) cold-rolled carbon steel prepared in accordance with Methods B or C of Methods D 609. 8. Conditioning and Number of Tests 8.1 Condition the test panels for at least 48 h at 23 2`( (73.5 3.5F) and 50 5 % relative humidity, and test in the same environment, or immediately on removal there from, unless otherwise specified or agreed upon by the sellei 3 The lester is available from BYK-Gardner, Inc.. 2435 Linden Lane, Silver Spring, MD 20910 or the Paul N. Gardner Company, Inc., 316 N.F.. First St, Pompano Beach, FL 33060. 986 mthe cd |owly pi| |te oftVj |m). IfT sivl FIG. DLJPO 50298164 D 5178 the purchaser. Test at least two replicate specimens of i material. procedure In preparation for using the apparatus, ensure that it is |sonably level and place it so that the weight holder is ard the operator. This places the beam release on the irator's right and allows freedom to move the test spec ial manually under the weighted scraping element (loop), lert the loop into the holder as far as it will go and tighten i clamping screw. Adjust the main bearing support so that 1 beam is balanced in the horizontal plane when the loop is it touching the specimen surface. The alignment of the gjm should be such that the end of the loop is over the lline of the movable table. FIG. 2 Balanced Beam Scrape Adhesion and Mar Tester ficirfs 1.2 Raise the beam and lock it in the raised position. Ipe the loop with a clean cloth or chamois. Locate the jcimemon the sliding platform against the stop so that the Jfcimen can be moved away from the operator and there is ||area at least 3 in. (75 mm) long by Vi in. (12 mm) wide on ; sample parallel to the horizontal plane through the beam. Ice weights on the weight support using an initial amount St is estimated to be appropriate for the particular coating. |lease the beam and carefully lower it until the loop rests ( the coated test specimen and the full load is applied, then (0.5-kg increments) until the coating is marred or until the maximum load of 10 kg has been applied. Use a new area of the test surface each time a scrape is made. 9.3 When the critical load has been approximately lo cated, repeat the test five times at each of three loadings: above, below and at the load determined in the first trial. Apply different loads in random fashion so that all scrapes at one load are not made in succession or on one panel. 9.3.1 Periodically examine the loop to ensure that the original smooth surface is intact. If the contacting surface is Jiwly push the sliding platform away from the operator at a ||e of Vi in. (6 mm)/s for a distance of at ieast 3 in. (75 worn, reverse the loop. When, both sides are worn, replace with a new loop. a). If the coating is marred, continue the testing using 9.4 For each applied load, tabulate the number of times lecessively smaller loads (0.5-kg increments) until the the coating was marred. fating is not marred. If the coating is not marred by the litial scrape, continue the test using successively larger loads 10. Report 10.1 Report the following information: 10.1.1 Load at the marring failure point, kg, 10.1.2 Panel material and surface preparation, 10.1.3 Dry-film thickness, and 10.1.4 Any deviation from the specified procedure. 11. Precision 11.1 Precision--If sufficient cooperators can be obtained, an interlaboratory study will be conducted to establish precision. FIG. 1 Balanced Beam Scrape Adhesion and Mar Tester 12. Keywords 12.1 balanced beam scrape adhesion and mar tester; balanced beam tester; coatings, mar or organic mar resistance The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such nghts, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your copiments are invited either for revision of this standard or tor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouid make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. h DUP050298165 # Designation: D 5179 - 91 Standard Test Method for Measuring Adhesion of Organic Coatings to Plastic Substrates by Direct Tensile Testing1 This standard is issued under the fixed designation D 5179; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method covers the laboratory determination oforganic coating adhesion to plastic substrates by mounting and removing an aluminum stud from the surface of the coating and measuring the force required to break the coating/substrate bond with a tensile tester. i .2 This test method requires that the aluminum stud be glued directly to the surface of a coated, cured panel (Fig. I). 1.3 This test method is used to compare the adhesion of coatings to various plastic substrates, thus allowing for a quantitative comparison of various coating/substrate combi nations. 1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility ofthe user ofthis standard to establish appro priate safely and health practices and determine the applica bility ofregulatory limitations prior to use. Aluminum Stud Adhesive r1 O Coating FIG. 1 Direct Tensile Model A-3/B" B-3/4" 0-5/16*' D-B/tS* 2. Summary of Test Method 2.1 An aluminum stud is bonded directly to a coated cured panel. The adhesive is allowed to cure for 2 h at room temperature. The specimen is then subjected to test on a tensile tester, equipped with an upper coupling adapter (Fig. 2), and a restraining device (Fig. 3). 3. Significance and Use 3.1 The pull-off strength (commonly referred to as adhe sion) of a coating is an important performance property that has been used in specifications. This test method serves as a means for uniformly preparing and testing organic coatings on plastic substrates.2 4. Apparatus and Materials 4.1 Tensile Tester, commercially available.3 4.2 Aluminum Stud--The shape and dimensions of the stud are shown in Fig. 1. 4.3 Upper Coupling Adaptor--The apparatus is shown in Fig. 2. The adaptor is 3% in. (94 mm) long, 1 >A in. (31 mm) in diameter at the top, and I in. (25 mm) in diameter at the 1 This test method is under the jurisdiction of ASTM Committee D-1 on Paints and Related Coalings and Materials and is the direct responsibility of Subcom mittee D0I.23 on Physical Properties of Applied Paint Films, Current edition approved Nov. 18, 1991. Published December 1991. 2 Gray, K. N., Buckley, S. E., and Nelson. G. L., "Assessing Measurement Standards for Coating Adhesion to Plastics" Modern Paint and Coatings Journal, Vol 75, No. 10, Oct. 1985* p. 160. 3 Tensile tester available from Instron Co., 300 Royal! St., Canton, MA 02021, or equivalent, has been found satisfactory for this purpose. rx FIG. 2 Upper Coupling Adaptor bottom. The hole, indicated by is used to attach the adaptor to the tensile tester load cell. The hole has a V2 in. (13 mm) diameter. The machined opening indicated by `VI." is to receive the head of the aluminum stud. 4.4 Restraining Device--The apparatus is shown in Fit 3 A and 3 B. The Vi-in. (13-mm) diameter hole, marked "a ," in the 2'/2-in. (63.5-mm) long, l'A-in. (31-mm) diameter lower coupling adapter, is used to mount the device in the tensile tester. The top portion is 4 in. (100 mm) in diameter, % in. (19 mm) high, and is fitted with a hole slightly larger than % in. (19 mm) in diameter to allow stud clearance. The bottom screw portion is machined to fit with the top portion and is V2 in. (13 mm) thick. Fig. 3 C illustrates the final appearance of the test assembly before it is tested. 4.5 Wooden Applicators,4 used to clean the adhesive from around the aluminum stud. * Applicators, such as Puritan available from 6 in. (150 mm) in length and 0.0? in. (2 mm) in diameter, have been found to be satisfactory for this purpose. 988 DUP050298166 A (3/4M diameter hole) PREPARED SAMPLE o eorron PQRS<o n -O SAMPLE AESIMlklNC o DEVICE FIG. 3 Direct Tensile Restraining Device Adhesive, cyanoacrylate adhesive.5 Since cyano4e adhesives loose adhesive bond strength with time, do se previously opened containers or lots of adhesive i to be old. Two-Kilogram Weight, approximately 2 in. (50 mm) ' meter and 5 in. (130 mm) in height. , r. reparation and Conditioning of Specimen Sanding Procedure--Sand large face of stud with sandpaper, making certain that the surface is uni'y roughened. When sanding studs, sand straight up and rotate stud one quarter of a turn and continue ng. Make certain surface-of stud is flat but rough! While ng, keep stud face 'parallel to sandpaper. Non-planar lees cannot be used in testing because they lead to aiform bonding of the stud to the coated surface. Only planar) studs should be used in testing. Planarity may be sed by placing a stud on a flat surface and checking to 'f the stud wobbles. Careful preparation of studs is tial for good adhesive adhesion. . Cleaning Procedure--Place sanded studs in a large r.'Pour technical gride adefone over the Studs and swirl V to completely vvasli' studs. Pour out acetone and t the cleaning prpeedure. Soak the stud for at least 15 1 pour out acetone, and allow stiids to dry. S' Place washed and dried studs and beaker in an oven at )C and allow to heat for 1 h. Remove the beaker and s from the oven and allow to cool. DO NOT TOUCH EOF STUDS. .4 Spread four drops of cyanoacrylate adhesive on the face of an aluminum stud. Next, quickly press the stud J .the coated test substrate. Place a 2-kg weight on the stud insure good contact between the stud, adhesive, and "ace of the coating. Clean the excess adhesive from the e of the stud with a wooden applicator. Carefully remove [.weight after 2 min. TU' 1--Substrate panels may be cut to any size that fits the !ning device. NVW' 2--When the'stud is pressed, excess adhesive should escape from under the stud. Excess adhesive buildup at the edge of the stud is a major source of error if allowed to dry. This excess must be removed from around the stud. The adhesive may he removed using a wooden applicator and an absorbent, creped, low-lint material.6 Some workers have found cotton swabs7 also work well when removing the excessive adhesive. 5.5 Allow the sample to cure for 2 h at room temperature. NXY' 2--When reusing aluminum studs, the studs must be soaked in acetone to remove coating and resanded. It has been found that soaking the studs in two separate acetone baths thoroughly removes the adhesive and coating. The first acetone bath is used to dissolve the cyanoacrylate adhesive, and the second is used to further clean and dissolve any coating or adhesive left on the stud. Before the studs are used, they should be resanded and cleaned with acetone as specified in 5.2, 5.3, and 5.4. 5.6 Conditioning--Condition the coated substrates for at least 24 h at 23 2C (73.5 3.5F) and 50 5 % relative humidity, and test in the same environment or immediately on removal therefrom, unless otherwise specified by the purchaser and seller. 6. Procedure 6.1 Install the restrainingtdevice and upper adaptor in the tensile testei;. . 6,2 Calibrate the tensile tester. Make sure that the chart speed is set at 8 to 20 in./min (20 to 50 cm/min). Make sure that the crosshead speed is set at 2 in./min (5 cm/min). Make sure that the chart full scale is set at 100 kg. 6.3 Place the specimen to be tested in the restraining device (Fig. 3 A arid 3 B). Pre-position the crosshead and then slowly lower it so the upper coupling adaptor can be attached to the test specimen. Take care to prevent the crosshead from impacting into the top of the specimen. Carefully attach the upper coupling adaptor to the stud (Fig 3 Q. NXY' 3--When testing thin substrates, a piece of plastic may be placed in the restraining device behind the test specimen to prevent the yanoacryiate adhesive such as Elmer's Wonder Bond Plus, or equivalent, has bund to be satisfactory for this purpose. 6 Kimwipes or equivalents, have been found satisfactory for this purpose. 1 Q-Tips or equivalents, have been found satisfactory for this purpose. D 5179 1TEST HG PROmm OATA SHEET 1OA (WE: Oats BAV TUB: Date NoTE-fi substrate from flexing when the stud is pulled from it. 6.4 Turn on the chart recorder and pen. Start the tensile test. Stop the test when the stress returns to zero on the chart. 6.5' Examine test area on each specimen to determine the type of coating failure, rating it according to the following; 6.5.1 Adhesive failure of the coating at the substrate. A, 6.5.2 Cohesive failure in the coating, C, 6.5.3 Combination of adhesive failure at the coating/ substrate interface and cohesive failure in the coating, AC, 6.5.4 Adhesive failure at the stud, S, and 6.5.5 Combination of adhesive failure at the stud and cohesive failure in the coating, CS. For multilayer coatings, note if the failure, is between the layers. If so, label as CM. 6.6 Number and retain all test specimens For adhesion failure calculations. Test five specimens of each coated substrate one day and five on a second day. If one specimen differs significantly from the other four at the same time, fails because of an uneven (non-planar) stud, or for any other reason performs unlike the other four, test a replacement specimen. NZ[' 4--Examine the stud and specimen carefully. Adhesive should have been applied uniformly to the entire stud surface. Coating should have pulled off uniformly over the entire stud surface either with adhesive failure from the substrate (A) or cohesive failure in the coating (C). If failure is less than 90 % A or C or (or CM), if the adhesive has ' failed at the stud, retest exercising particular care in the specimen and stud preparation. N\]' 5--The percentage of adhesive failure at the coating/substrate interface is determined by inspecting the tested area on the substrate. This may be assessed by overlaying a transparent sheet grid marked in 0.10-in. (2.54 mm) squares and estimating the percentage of adhesive 1 -i failure in each square that lies over the tested area. These percental., may then be averaged to obtain failure for each specimen. tL N^_' 6--Sample conditioning, ifany, and humidity and tempei .win: of test room may affect results. Notation of these conditions should 1 made on the test report. 1 7. Report ; 7.1 Report the number of tests, the maximum si (9 obtained in each test, and the type of failure. Test data-sheet.* is shown in Fig. 4. Fill in data sheet with results obtained from each test. Attach tensile test traces to.the data sheets^ Calculate and report mean and standard deviation for tensilS'j'-i strength for each coating/substrate combination tested. 8. Precision and Bias8 8.1 The precision and bias are primarily dependent upon'; the accuracy ofthe force measurements, the alignment of the ; device, the. cafe exercised urslud and specimen preparation,; and the care in testing. 8.2 A round robin involving five different types of coat- j ings and seven different plastic substrates, and te,n different; laboratories yielded interlaboratory reproducibility data as; shown in Table 1. Within laboratory repeatability data -s shown in Tables 2 and 3. 9. Keywords 9.1 adhesion; bond strength; cyanoacrylate adhesive; plastic substrate; pull-off strength; pull testing; tensile tester 8 A complete teport with additional data is available. See Nelson, G. 1~ "Testing of EMi/RFl Coating Adhesion to Plastics by a Tensile Test Method,1'; Final Reportfor Computer and Business Manufacturers Association and Society 0/ the Plastics Industry, University ofSouthern Mississippi, June, 1989. :Labbc \* Labpfj.. Labor!:. NOTEw--li> gamble ` Numoer] 990 DUP050298168 # D 5179 TABLE 1 Overall Test Reproducibility N`a' --This data was generated with lesser cautionary language than found in Note 2 and includes laboratories who had not removed excess adhesive. With experienced operators, reproducibility data can be anticipated to be- better than shown In Table 1. Ten Laboratories Sample Kilogram Force Standard Deviation 1 34.6 6.7 2 36.2 9.3 3 19.8 4.5 4 26.7 8.7 5 31.7 9.9 6 26.0 7.2 7 41.6 9.2 8 16.6 6.5 9 60.5 20.5 10 28.3 9.6 TABLE 2 Average Tensile Strength Measurements4 n o t ' --Units for tensile strength and standard deviation are kilograms of force. Multiply by 4.99 to convert to pounds per square inch. r* Sample Number 1 2345678 vf Laboratory 1 X 33.2 32.2 iv SDS 4.3 4.6 t" Laboratory 2 X 29.2 30.9 SD 5.5 5.8 Laboratory 3 X 33.5 35.7 SO 7.0 4.4 W Laboratory 4 X 41.9 45.1 rcenlages W`i1 Laboratory 5 SD X 10.4 4.8 27.5 23.0 SD 1.1 2.0 lperaturc Laboratory 6 X 42.4 >41.9 ihoukl he SD 6.7 5.2 * Laboratory 7 X 42.6 42.0 SD 4.1 . 10.0 Laboratory 8 X 23.2 30.9 2 stress , E; Laboratory 9 ta sheet SD X SD 5.6 5.1 34.0 26.4 8.4 8.2 btain&fy i Laboratory 10 sheets, X SD 36.9 53.4 9.9 6.5 r tensile id. A Each is average tensile strength using ten samples. B' Standard deviation. 12.9 2.2 19.9 2.8 24.2 3.9 26.2 6.1 18.7 3.7 26.2 3.0 19.0 2.4 18.6 4.8 16.2 8.8 17.6 28 23.5 3.5 28.0 3.7 32.2 11.8 31.8 7.6 19.3 2.2 31.6 4.8 29.4 3.7 8.6 1.8 25.6 7.6 41.8 8.7 25.3 10.6 33.9 9.2 33.8 5.4 43.2 6.4 24.3 4.0 48.3 6.7 31.9 5.0 20.6 4.7 17.4 2.5 38.5 10.2 20.8 3.8 22.3 6.3 31.2 6.4 37.2 7.7 21.1 2.5 34.1 3.5 28.9 4.7 21.8 7.7 13.9 5.3 28.5 9.2 38.8 6.3 36.8 7.5 49.8 9.5 50.5 8.8 32.1 5.3 53.1 11.7 45.8 9.9 32.8 9.7 27.1 8.8 49.3 7.4 5.8 2.1 9.1 4.0 18.6 4.5 17.2 5.8 26.4 14.3 23.9 6.5 16.8 9.5 19.8 7.5 10.4 5.5 18.1 8.5 9 63.9 12.2 B0.3 10.7 79.1 9.6 >72.7 18.7 44.6 11.1 >65.2 4.8 72.4 26.1 32.1 6.2 36.6 12.4 36.4 14.9 10 21.8 2.5 26.0 5.7 39.7 7.2 33.0 9.4 19.9 3.1 33.7 2.2 37.3 6.3 11.2 2.6 20.8 5.B ' 40.0 9.0 it upon it of the iratipn, jf coat ifferent! data; a? data is j Ihesive; tester j, G. L., Method," Society of \ f TABLE 3 Average Tensile Strengths, Standard Deviations (SD) and Ranks *-Nbc' --Units for tensile strength and standard deviation are kilograms of force. Multiply by 4.99 to convert to pounds per square inch. ijl?. Sample ji Number Coaling Substrate Failure Mode Average Collaborator A SD Rank '-- Average Collaborator B' -- SD Rank fit 1 1K z3 H4 m5 K6 ft 7 18 I9 H 10 1 11 If 12 13 I 14 1 15 Lacquer Lacquer Lacquer Lacquer Lacquer Lacquer Enamel Urethane Urethane Urethane Enamel Lacquer Enamel Enamel Enamel Xenoy* Lexan5 ABS polycarbonate ABS PVC polycarbonate ABS ABS metal metal GTX 901 GTX901 GTX 901 GTX 901 c 10.7 A 5.8 C 10.2 A 5.4 C 12.6 AC 15.4 A 55.6 A 133.5 A 98.9 S 133.7 AE 61.6 c 27.8 c 24.7 A 40.9 A 34.6 3.8 1.0 0.8 2.7 3.4 3.3 29.1 23.6 12.4 46.1 14.8 4.9 6.8 14.1 10.4 12 14 13 15 11 10 5 2 3 1 4 8 9 6 7 12.5 8.8 22.8 9.6 24.8 25.9 67.7 122.5 91.7 133.4 75.4 62.9 66.0 56.0 50.6 2.5 2.4 3.8 1.9 4.5 3.1 9.5 24.9 16.9 51.5 14.3 6.8 17.9 14.6 19.1 13 15 12 14 11 10 6 2 3 1 4 7 5 8 9 * Polycarbonate-based polymer alloy is a trademark of the General Electric Co. * Polycarbonate resin is a trademark of the General Electric Co. - , - ABS = acrylonitrile butadiene styrene. 0 PVC = polyfvinyl chloride). ' e Failure rate is 75 %. 991 ! Ph DUP050298169 (5 0 5179 TheAmerican Society for Testing andMaterials takas noposition respecting the validity of any patent rights asserted In connection with any Item mentioned In, this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility.. This standard is subject to revision et any time by the responsible technical commktea and must bs reviewed every five years and ifnot revised, either reapprovedor withdrawn. Tour comments are invited either forrevision ofthis standard ortoradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a lair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. 992 DUP050298170 Designation: D 5181 - 91 Standard Test Method for Abrasion Resistance of Printed Matter by the GA-CAT Comprehensive Abrasion Tester1 This standard is issued under the fixed designation D 5181; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon <<) indicates an editorial change since the last revision or reapproval. Scope JR 1 This test method covers the procedure for determining 11 abrasion resistance of printed matter using a GA-CAT prnprehensive Abrasion Tester. gO This test method is applicable to packaging labels, |k, catalog, and magazine covers, bar codes, corrugated Res, and other containers having applied graphics on any j| substrate. if.3 This standard does not purport to address all of the Wely problems, if any, associated with its use. It is the jMonsibility ofthe user ofthis standard to establish appro'I mle safety and health practices and determine the applicatf.ity ofregulatory limitations prior to use. ' p'-Referenced Documents lf|2.1 ASTM Standards: J PE 171 Specification for Standard Atmospheres for Condi$ r tioning and Testing Materials2 * U Terminology P3.1 Definitions of Terms Specific to This Standard: fS.1.1 abrasion resistance--resistance against the act of Heaping, smudging, or rubbing off. ' 3.1.2 abrasiveness--the degree to which a product tends M cause abrasion by the act of rubbing or scraping. , 3.1.3 receptor--film or paper of standard abrasiveness Ipnto which material removed from the specimen is deposited .^hiring the abrasion testing process. Alternatively, printed _ caper from which material is removed onto the specimen ghat has a higher degree of abrasiveness than the receptor (in case of testing abrasiveness). L Summary of Test Method i | 4.1 The test print and a receptor are sandwiched in the ^pancl holder of the GA-CAT Comprehensive Abrasion | pester, clamped together with a known force, and made to slide over each other at a known frequency and over a Known distance for a predetermined time period, jg 4.2 The test specimen is examined for degree of print ^degradation and the receptor for amount of ink or other " terial transferred from the specimen surface. Results may rated relative to a comparative control run in the identical inner, or they may be quantified by comparison to a This test method is under thejurisdiction of ASTM Committee D-I on Paints Related Coatings and Materials and is the direct responsibility of Subcomittee D01.56 on Printing Inks. Current edition approved Oct. 15, 1991. Published December 1991. 2 Annual Book ofASTM Standards, Vols 08.03 and 15.09. ranking scale numbered from zero to ten (zero being the most abrasion resistant and ten the least abrasion resistant). 5. Significance mid Use 5.1 Abrasion resistance during transport and storage is essential to prevent marring of type matter, designs, or protective coatings on the exterior oflabels and other printed materials. Recognizing that the actual amount of abrasion occurring in the field depends on relative humidity, temper ature, tightness pf packing, and a host of other variables, this test method provides a rapid means for comparing the abrasion resistance of test surfaces under laboratory condi tions. It is useful for specification acceptance between the supplier and the customer. 5.2 This test method can also be used to evaluate the relative abrasion resistance of printed inks, varnishes, lami nates and substrates, and the abrasiveness of inks. 6. Apparatus 6.1 GA-CAT Comprehensive Abrasion Tester.3 6.2 Ranking Book3 containing specimens whose degree of nibofF is ranked from 0 (no rubofi) to +10 (most ruboff). 7. Materials 7.1 Standard Receptors, approximately 4 by 4 Vi in. (102 by 114 mm), of an appropriate grade, as follows; 7.1.1 C-P (least abrasive)--Glossy coated paper suitable for use with samples of low abrasion resistance. 7.1.2 A-l, A-3, and A-43-4 (intermediate abrasiveness)-- Imperial lapping film with aluminum oxide abrasive parti cles of different sizes (9, 12, and 30 pm, respectively). 7.1.3 A-63-4 (most abrasive), wet or dry, tri-um-ite 600. 7.1.4 B-23 (intermediate-abrasion resistance)--Printed single color paper suitable for measuring abrasiveness of samples of average abrasiveness (corrugated). Nde' I--Other receptors may be substituted provided they have equal abrasiveness on the same test specimens. Further research and experience may indicate a need for additional grades of standard receptors. 7.2 Foam Sheeting3 2 pieces, each approximately 2 mm in thickness and cut to 4 by 4*/2 in. (102 by 114 mm). Nde' 2--Use of foam sheeting as a backing for the test specimen and the receptor is recommended to provide uniform pressure over the test surfaces and to prevent ink, varnish, or other particles from becoming imbedded in the sensitive surface of the panel holders. 3 Available from Gavarti Assoc., Ltd, 9240 N. Sleepy Hollow Milwaukee, W! 53217. 4 Available from 3M Co., St. Paul, MN 55119. 993 DUP050298171 D 5181 7.3 Comparative Control, a production or laboratory print preferably having known abrasion resistance. The compara tive control must have the same substrate, color(s), and subject matter as the test print. 8. Test Specimen and Conditioning 8.1 The specimen size in the grain direction (or flute in the case of corrugated board) must not exceed 4l/> in. (114 mm). The specimen size in the cross-grain direction is less critical; 4 in. (102 mm) is recommended. Care should be taken to avoid contaminating the test surface with finger prints during specimen cutting and handling. 8.2 Condition the specimens at 73.5 3.6F (23 2C) and 50 5 % relative humidity in accordance with Specifi cation E 171. 9. Preparation of Apparatus 9.1 Set the abrasion tester on a sturdy bench, preferably in a room conditioned at the temperature and relative humidity prescribed in 8.2. Make sure that the three-prong power cord is correctly connected, 9.2 Periodically, check the liquid level in the hydraulic pressure system. If not full, follow the instructions in the manufacturer's manual 9.3 If test conditions have not been specified, select an appropriate receptor by running the reference standard for the length of time required to achieve a visible level of degradation. Start with receptor C-l (7.1.1). If the test time exceeds 2 min, use a receptor with a higher level of abrasiveness. Nfg' 3--Excessively long rubbing times are to be avoided because they introduce uncontrollable heat development that can alter the results. 10. Procedure for Abrasion Testing 10.1 Loading the Instrument: 10.1. i Move the tray containing the four panel holders to the front black support shelf. Make sure that the inscribed "L" appears on the upper left side ofthe left panel holder and the "R" in the upper right side of the right panel holder (see Fig. 1). There should be space of at least V?. in. between the two center panel holders. 10.1.2 Face the test specimen on the receptor (selected in 9.3) and sandwich between the foam sheets. Place the sandwich between the two center panel holders so that the Place Test Panels Here Spacer Panels Protective Foam Sheets FIG. 1 Panel Holders Test Print grain direction of the specimen is vertical Take care that ft > sandwich does not extend below the bottom of the panel holders. 10.1.3 Push the four panel holders together into an upright parallel position. Make sure that the sandwich is not pinched at the bottom of the panel holders; otherwise, it yj]j, tend to slide down during the test. Grab the pins and move the tray inside the instrument so that the two retaining pins drop into the carriage holes. If the pins do not drop into th. n respective holes, recenter the panel holders on the sample tray. 10.1.4 Apply side pressure by turning the lower black spindle until the corresponding dial reads 20 pounds per square inch (psi). Do not apply top pressure'at this time. 10.1.5 The carriage inside the instrument is meant move between two limit switches (used for centering proximately 2 in. (50.8 mm) apart. If the carriage is not if situated between these limits, manually center the carriage ' 10.2 Testing Under the Preset Mode: 10.2.1 Turn the power switch on by pressing the upper side of the flip switch at the right side of the instrument. 10.2.2 After the control box window (LCD) displs "GA-CAT ready," press CNTR; the LCD will read "Check limits" to make sure the carriage is within the range of the limit switches. Press CNTR again and the LCD will read "release top pressure." Press CNTR once more and the carriage will move to the extreme right (limit switch) and then back to stop exactly in the center. At this poinl, the LCD will show that the carriage has been centered ly showing a flashing square after "GA-CAT READY." 10.2.3 After the instrument is centered, apply the tn pressure of 40 psi. 10.2.4 Push the "STRT" button. The LCD will read "computing" and after 3 s, the instrument will run under the following default values: Time S.O s Frequency 2.0 Hz Span 1.0 in. Offset 0.0 in. 10.2.5 When the instrument stops, release the top pres sure, making sure that the top pressure plate is high enough to clear the panel holders. Push CNTR to re-center the carriage. Release the side pressure and pull the panel holders out of the carriage. Remove the sandwich and examine the test specimen and the receptor. 10.2.6 To continue running the test with the same set tings, reload the instrument as in 10.1, apply the top pressu . as in 10.2.3, and push STRT. When the instrument stops follow the procedure in 10.2.5. Turn the switch off only at the conclusion of testing. 10.3 Changing the Default Values: - 10.3.1 The default values may be changed to any of the following settings; Time Frequency Span Offset Continuous from 1 to 3600 s 0.2 to 3.0 Hz (cycles per s) with a resolution of 0.! Hz 0.1 to 1.9 in. with a resolution of 0.1 in. 0.1 to 0,4 in. (increments of 0.1 in.) 10.3.2 In order to change a setting, press the "mode" button until the LCD displays the default value to be altered. Enter the new value on the number buttons and then press "enter." The LCD will read "new value?". If the value is correct, press "enter" a second time. If incorrect, enter jfc-Iothe om ze; Esped .y; 994 i ' t- DUP050298172 5 that the Hither value or press "clear" and start over again. 12. Precision and Bias he panel into JflpTE 4--The instrument reverts to the original default values by "reset" and any time the instrument is turned off. 12.1 Precision--An interlaboratory study of this test method was conducted in which operators in 17 laboratories tested six prints in triplicate on each of two days. The prints eh is nL! 3e, it v ad raov ling pins nto then ! saittj 0.3.3 When running thick samples such as corrugated iterial, follow the procedure in 10.1 through 10.2.1. If the `:er of the panel holders is not aligned with the center of the carriage, use the "offset" mode. Press the , node" button until "offset" appears and then enter the new j! fitting. A setting of 0.1 or 0.2 is recommended. An addi- consisted of three density levels of two different colors and were ranked for abrasion resistance from 1.0 to 4.0. The within-laboratory pooled standard deviation was 0.54 at 15 df and the between-Iaboratories pooled standard deviation was 0.58 at 18 df. Based on statistical analysis of the results, the following criteria should be used for judging the accept imal adjustment for overall width of the panel holders may ability of results at the 95 % confidence level: sr blaoi mds f m be necessary by removing one or two black separators. fo.3.4 Proceed further as in 10.2.2 until 10.2.6. 12.1.1 Repeatability--Two results, each the mean of two determinations obtained by the same operator on different time; days, should be considered suspect jf they 'differ by more leant than 1.5 ranking units. mg) ap- Interpretation of Results 12.1.2 Reproducibility--Two results, each the mean of e is not image. e upper lent, |l. 1 Run the test material and the comparative control in gw! identical manner. Examine each print for degree of Jegradation and each receptor for amount of material feinsferred from the print. Report results for abrasion itive to the comparative control as equal, slightly or results obtained on different days by operators in different laboratories, should be considered suspect if they differ by more than 2.2 ranking units. 12.2 Bias--Bias cannot be determined as there are no standard materials. displays, "check e of tfie' ill read tnd the- jjpreciably less, or slightly or appreciably greater. '1.2 A numerical record of degree of abrasion ranging !m zero to ten can be obtained from a comparison of the I specimen with examples in the Ranking Book (6.2). 13. Keywords 13.1 abrasion; abrasiveness; printed matter; printing inks; smudging :h) and int, ih The American Society for Testing and Material takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such :red by patent rights, and the risk of infringement of such rights, are entirely their own responsibility. :he lop 11 real derlhe , This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or, withdrawn. Your commentsare invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. tlie iers the essure stops, inly at of the 995 DU P0502 98173 <1 Designation: D 5200 - 91 Standard Test Method for Determination of Volatile Organic Compounds (VOC) of Solvent Reducible Paints in Aerosol Cans1 This standard is issued under the fixed designation D 5200; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number tn parentheses indicatesthe year of last reapproval, superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This test method is for the determination of the volatile organic compounds of solvent-based patients in aerosol cans. It offers a unique way to obtain paint speci mens from aerosol cans. 1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user ofthis standard to establish appro priate safety and health practices and determine the applica bility ofregulatory limitations prior to use. A specific hazard statement is given in Note 1. 2. Referenced Documents 2.1 ASTM Standards: E 145 Specification for Gravity-Convection and Forced- Ventilation Ovens2 E 180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemicals3 Glass Wool 3. Summary of Test Method 3.1 A designated quantity from an aerosol coating is sprayed into an adapter glass tube assembly and heated in an oven at 110 5C for 60 min. The percent volatile is calculated from the loss in weight. 4. Significance and Use FIG. 1 Adapter Glass Tube Assembly 4.1 This test method is the procedure of choice for determining volatiles in coatings for the purpose of calcu. fating the volatile organic content in aerosols under specified test conditions. The inverse value, nonvolatile, is used to determine the weight percent solids content. This informa tion is useful to the paint producer, user, and to environ mental interests for determining the grams of volatile organic compounds per gram of solids emitted from aerosol cans. 5. Apparatus precondition for 30 min in an oven at 110 5C and stor< in a dessicator prior to use.4-- 5.1.2 Charcoal Adapter Tube, straight connecting with 35/25 spherical joints. Fill -with activated charcoal and plug both ends with glass wool. This tube is used to prevent the solvent vapors from contaminating the vacuum pump.5 6 5.1.3 Adapters, connecting hose with 35/25 socket joints.' 5.1.4 Adapter,7 connecting hose with 35/25 ball joint. 5.1.5 Clamps, pinch type, with screw locking device.8 5.1 Adapter Glass Tube Assembly, (Fig. 1). 5.1.1 Sample Adapter Tube, straight connecting with 4 Sample adapler tube, Catalog No. 5035-35, available from Ace Glass Inc., 35/25 spherical joints. Loosely fill with glass wool and P.O. Box 668, 1430 Northwest Boulevard, Vineland, NJ 08360, has been found suitable for this purpose. 5 Charcoal adapter tube, Catalog No. 5035-3, available from Ace Glass Inc. has been found suitable for this purpose. `This test method is under the jurisdiction of ASTM Committee D-01 on 6 Adapters (socket joints). Catalog No. 5217-35, available from Ace Glass Inc. I Paints and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.21 on Chemical Analysis of Paints and Paint Materials. have been found suitable for this purpose. 7 Adapter (ball joint), Catalog No. 5216-35, available from Ace Glass Inc. has Current edition approved Nov. 18, 1991. Published December 1991. been found suitable for this purpose. 2 Annual Book ofASTM Standards, Vo! 14.02. 8 Clamps, Catalog No. 7669-14, available from Ace Glass Inc. have been found * Annual Book ofASTM Standards, VoJ 15.05. suitable for this purpose. 996 DUP050298174 6 Glass Wool, medium fine silk. 7 Activated Charcoal, cocoanut, 8 to 12 mesh. 8 Tygon Tubing. 9 Iron Stands. '10 Utility Clamps. \ Vacuum Pump. kForced Draft Oven, Type IIA or Type IIB as specified eification E 145. I Actuators (Valves), with extension tubes. ' Top Loading Balance, capable of weighing to 0.01 g. ; Shaker, similar to the Eberbach shaker in Fig. 2. cedure Mix the aerosol can thoroughly using a shaker, similar Eberbach shaker in Fig. 2, For 15 min at the low speed , It is essential that the samples be well mixed Jo valid results. Weigh accurately to 0.01 g, a preconditioned sample pc tube. Use a pair of gloves at ail times when handling 'dapter glass tube. Remove the cap and actuator from the mixed can. ce the actuator with one having an extension tube. Test actuator and extension tube fit by spraying some nts out for about 5 s.. This step also clears the dip tube a separation has occurred. If a leak is observed, ce with a better fitting actuator or extension tube. Weigh the aerosol can with the actuatoT to the nearest j. Spray 3 to 5 g of aerosol into the adapter tube bly, spreading out the coating by moving the extension around the wall of the adapter tube, The spraying is with the vacuum on. Obtain the specimen weight by difference by weighing aerosol can again to 0.01 g after spraying out the imen. 6.7 Place the sample adapter tube in the drying oven for 60 min at 110 5C. Nij' I: Warning--Provide adequate ventilation, consistent with accepted laboratory practice, to prevent solvent vapors from accumulating to a dangerous level. 6.8 Remove the adapter tubes from the oven, place immediately in a dessicator, cool to ambient temperature and weigh to 0.01 g. 7. Calculations 7.1 Calculate the percent nonvolatile NV, in the aerosol can as follows: NV, % = (W2/W,) X 100 . / (1) where: W, = weight of aerosol can before spraying sample minus weight of aerosol can after spraying sample, g, and W2 = weight of sample adapter tube with solids minus weight of sample adapter tube, g. 7.2 The percent volatile organic compounds, VOC in the aerosol can may be calculated by the difference as follows: VOC, % = 100 - NV (2) where grams of VOC/grams of solid equal VOC/NV. 8. Precision and Bias 8.1 Precision--Estimates are based on an interlaboratory study in which 1 operator in each of 3 laboratories analyzed in duplicate on two different days 3 samples of solvent-based aerosol coatings containing 63.04 % to 77.53 % VOC. The coatings were commercially supplied. The results were ana lyzed statistically in accordance with Practice E 180. The within laboratory coefficient of variation was found to be 0.51 % relative at 9 df and the between laboratory coefficient of variation was 1.04 % relative at 6 df. Based oh these coefficients the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 8.1.1 Repeatability--Two results, each the. mean of dupli cate determinations obtained by the same operator on different days, should be considered suspect if they differ by more than 1.62 % relative. 8.1.2 Reproducibility--Two results, each the mean of duplicate determinations obtained by operators in different laboratories should be considered suspect if they differ by more than 3.59 %. 8.2 Bias--Bias has not been determined. TheAmerican Society for Testing andMaterials takes no position respecting the validity ofanypatent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision ai any time by the responsible technical committee and must 6s reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feet that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7916 Race St., Philadelphia, PA 19103. ft ! s * > sf iE 997 DUP0502981 75 Designation: D 5201 - 91 Standard Practice for Calculating Formulation Physical Constants of Paints and Coatings1 This standard is issued under the fixed designation D 5201; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This practice describes procedures for calculating weight solids, volume solids, solvent content, and density of liquid paints and coatings based on formulation data (not from analytical determinations). These calculations may be related to either as-supplied (unreduced) or as-applied (re duced) coating materials, including multicomponent types. 1.2 These values may not be acceptable for regulatory gurposes. 1.3 Calculated values for these physical constants are used in the coatings industry for developing lower volatile organic compound (VOC) paints, making comparisons, etc. 1.4 The calculations described in this practice are based on the following assumptions: (1) Solids (nonvolatile) con tent and density of the individual ingredients (raw materials or intermediates, or both) have been established by appro priate analytical methods (see Test Methods D 153, D 1475, D2369, D 4558, and Guide D 2832), and (2) The blended formulation behaves as an ideal solution with no volume change on mixing (see 6.2). 1.5 In calculations involving the liquids in a formulation, those volatile liquids that are incorporated primarily for vehicle solvency and control of the application characteris tics should be classified as solvents. This would include solvents normally used to adjust viscosity for application and appearance of the coating. Liquids that are expected to be retained in the dried film to affect the final performance properties should be classified as part of the coating solids. No t ' 1--For regulatory VOC purposes, use EPA Reference Method 24 and ASTM standards listed, or state regulatory requirements (see EPA 450/3-88-018). 1.6 Volatile by-products of cross-linking reactions (cure volatiles) are not considered in;these calculations since the object of this practice is to define paint physical constants based on formulation information. 2. Referenced Documents 2.1 ASTM Standards: D 153 Test Methods for Specific Gravity of Pigments2 D1475 Test Method For Density of Paint, Varnish, Lacquer, and Related Products3 D 2369 Test Methods for Volatile Content of Coatings3 D2832 Guide for Determining Volatile and Nonvolatile! Content of Paint and Related Coatings3 I D 3960 Practice for Determining Volatile Organic Com-I pound (VOC) Content of Paints and Related Coatings3! .D4558 Test Method for Nonvolatile Content of Latexes2! 2.2 U. S. Environmental Protection Agency Standards: EPA 450/3-88-018, U.S. Environmental Protection! Agency Protocol for Determining the Daily Volatile Organic Compound Emission Rate of Automobile and! Light Duty Truck Topcoat Operations4 EPA Federal Reference Method 24--Determination of; Volatile Matter Content, Water Content, Density, Volume Solids, and Weight Solids, of Surface Coatings5! 3. Terminology 3.1 Description of Terms Specific to This Standard: `` MS 3.1.1 formula 'density--(see Test Method D 1475), the mass (weight in vacuum) of a unit volume of material at any given temperature. 3.1.1.1 kD< ( lkk< mn--In this practice, density is expressed in pounds per U.S. gallon (lb/gal) since this is commonly used in the coatings industry. Where dry materials an. concerned, actual density (not bulk density) should h' determined analytically or obtained from supplier informa tion. Use Test Methods D 153 where applicable. 3.1.2 formula percent volume solids content--the calcu lated volume of nonvolatile material in a formula divided by the total volume of the paint material, times 100 %. 3.1.3 formula percent weight solids content--the calcu lated weight of nonvolatile material in a formula divided t\ the total weight of the-eoating material, times 100 %. 3.1.4 formula solvent content--the calculated weight ot the solvents in a specific volume of paint (such as pounds of solvent per gallon of paint) based pa formulation, which is determined by totalling all solvents present. 3.1.4.1 nD< ( onn< pq--Volatile by-products of cross-linking reactions (cure volatiles) are not included in the formula solvent content. See Note 1 and applicable government regulations for definition of the term VOC. 3.1.5 formula solvent density--the calculated density of the combined solvent composition. 3.1.6 formula VOC content--calculated amount based 1 This practice is under the jurisdiction of ASTM Committee D-l on Paint and Related Coatings and Materials and is the direct responsibility of Subcommittee DO 1.24 on Physical Properties of Liquid Paints and Paint Materials. Current edition approved Nov. 15, 1991. Published January 1992. 2 Annual Book ofASTM Standards> Voi 06.02. 3 Annual Book ofASTM Standards, Vol 06.0 i, 4 Available from Superintendent of Documents. U.S. Government Printing Office. Washington, DC 20402. Refer to EPA 450/3-R8-018 dated December 1988. This protocol makes reference to the paint formulation physical constants for VOC and volume solids content. 5 Available from Superintendent of Documents, U.S. Government Printing OJfice, Washington, DC 20402. 998 f `I;. DUP050298176 # D 5201 total formula solvent content, (such as pounds of ent per gallon of paint) exclusive ofwater of solvents that lexempted by regulations. This is a theoretical value. 11,6.1 rD< ( srr< tu--Solvent and VOC are not equivalent volatile to Cotn- ; ratings3 -atexes2 ,, ards: otection Volatile Dile and ition of Density .. Datings5 i: '5), the 1 at any ' pressed imonly als are i uld be 1 iforma- lj ii! caicu- ' ided by :|| caicu-. .! ded by ight of mds of hich is linking irmula nment sity of based Significance and Use ; 1 Physical constants of paints and coatings are required [ aspects oftheir formulation, manufacture and use. This itice demonstrates standard methods agreed upon for ulating formulation values for some of these physical jstants. The calculations are the same for either metric or h/pound units. These formula values may not be used to replace insured values required by government regulations unless ieifically stated in the governing documents. Calculations ;.L Formula Density (weight per unit volume): .1.1 The formula density (Z>f) can be calculated from the weight {We) and total volume (Vr) of the formulation. : formulation volume can be calculated from the weight density of each ingredient as given by the following atiom Ws X W./D, + W2/D2 + ... WJDn w; WVA 0) here: = number of items in the formulation, = formula density, Ib/gal (g/L), = total weight of formula, lb (g), ' 1 = total volume of formula, gal (L), = weight of ingredient, lb (g), and = density of ingredient. 5.1.1.1 An example would be as follows: I Ingredient Weight W, (lb> Density D, (lb/gal) Volume V, (gal) Simula 81.50 7.74 10.530 6.10 7.90 0.772 0.40 8.72 0.046 12.00 7.65 1.569 100.00 Dr 12.917 100 (lerefore, formula density, Dr = ^ 9(7 = 7.74 lb/g'al. 15.1.2 The density of any one of the1 ingredients in a tppduct can be calculated as long as the density of the paint Simulation and the other ingredients in that formulation are ppwn (D = W/ V), as in the following example: .. Igrediem Weight w, (lb) Density D, (lb/gal) Volume v, (gal) plymer sblids .divent A |lvent B prmula 50.00 25.00 25.00 100.00 DpS 6.95 7.18 7.50 3.60 3.48 V, Printing )sr]988. for VOC Printing Where: = volume of total formula, gal = 100.00 = 13.3 _ = volume of polymer solids, gal = 13.33 -- (3.60 + 3.48) = 6.25 gal, and Dps= density of polymer solids, Ib/gal = 50.00 6.25 = 8.00 lb/gal. 5.2 Formula Solvent (Volatile) Density: 5.2.1 The density of the solvent (volatile) portion can be calculated using the following equation: D V>D' + VA + K3A + VnDr, . ViDl ! V + v2+v2 + ...va . V, (2) where: D,, - density of solid formula, lb/gal (g/L), Vj = volume of solvent, gal (L), D\ = density of solvent, lb/gal (g/L), and n = number of items in the formulation. . 5.3 Formula Weight Percent Solids (Nonvolatile): 5.3.1 Calculate percent of solids by weight as follows: weight of solids 5L = - x 100 total weight of coating (3) where S,,, = weight percent of solids (nonvolatile), %. 5.4 Formula Volume Percent Solids (Nonvolatile): 5.4.1 Calculate percent of solids by volume using either of the following equations depending on available information: volume of solids x 100 total volume of paint (4) where Sv < volume percent of solids (nonvolatile), %. or, 5.4.1.1 Generally the volume solids content is calculated by subtracting the volume of all solvent from the total volume since the volume of the solvent portion is' usually more readily available than the'volume of solid materials total volume of paint - volume ofsolvents ... Sv ---------------------- ---------- 4---------------------- x 100 (5) total volume of paint where Sy = total volume percent of paint minus volume of solids. 5.4.2 When the volume solids of each ingredient in a formulation is known, the volume solids of the formulation can be calculated. 5.4.2.1 The volume IT'D of each ingredient is calculated from the formula weight (WJ of each ingredient divided by its density (D{). V\ = WyD, (6) 5.4.2.2 Total volume of the formula is determined by the sum of the volumes of the individual ingredients Vr^ZV (7) 5.4.2.3 Formula volume solids (S'vf) is calculated in the following manner. The volume of each ingredient (Pi) is multiplied by the volume percent solids of that ingredient (SJ and the sum of these volume solids is divided by the total volume of the formula to give formula volume solids. This is shown symbolically as follows: ,, Svf~ Xn yt (8) 999 DUP050298177 D 5201 5.4.2.4 An example would be as follows: gredient Weight Density Total Volume W, (lb) D, (lb/gal) Volume Solids, % 1 7.35 8.00 0.92 31.0 2 22.41 7.96 2.82 21.5 3 52.85 8.24 6.41 23.8 4 5.98 7.16 0.84- 0.0 5 6.13 9.27 0.66 100.00 6 0.28 7.17 0.04 0,0 7 -5.00 8.14 -Ml 33.6 100.00 12.30 it volume of solids, gal X 100 total volume, gal 3.29 x 100 = 26.7 ' 12.30 Volume of Solids 0.29 0.61 1.53 ... 0.66 m 3.29 (9) 5.5 Formula Total Solvent Content and VOC Content (see 3.6): " 5.5.1 If all ofthe solvent in, the formulation is considered to be VOC for regulatory purposes, the VOC content may be expressed- as pounds of VOC per gallon (grams per litre) of paint material,: calculated as follows: VOC (Ib/gal), (100 - weight( solids) x density of coating 100 (10) . 5.5.2 If water is present in the paint material formulation, it must be subtracted from the total volatile portion in determining the formulation VOC content VOC (Ibs/gal) (less water) -- weight of volatiles -- weight of water volume of paint *- volume of water , or, (100-weight percent of solids - weight percent of water) formula density (weight percent of water) formula density 100- water density (11) where- density equals pounds/gallon (grams per litre). Nvw' 2--Deduction for other non-VOC volatile ingredients as defined in local ordinances may be treated in a manner similar to water as just illustrated and in Practice D 3960. ' Nxy' 3--Solvent content and VOC content values maty be converted from pounds per (U.S.) gallon (Ib/gal) to grams per litre (g/L) by multiplying by tl9.84. 5.6 Paints Reducedfor Application: 5.6.1 The calculations and examples shown in 5.1 through 5.5 are for as-supplied materials intended for use without further reduction. The same calculations can be used for determining the formulation density, percent weight solids content, percent volume solids content, and solvent (VOC) content of materials that have been reduced for application. It is only necessary to know the amount of reduction (volume or weight) and the density of the reducing solvent. The reducing solvent then becomes an additional ingredient in the paint formulation. 5.6.2 Each of the following examples is based on jjequation: w D =-- V where: D = density, W = weight, and V = volume. 5.6.2.1 Density of Reduced Material Knowing PerKK, Reduction by Volume: * ' (1) The paint material described in the example in 5.1,[.i'' is'reduced 20 % by volume with reducing thinner having a.I density of 7,20 Ib/gal as follows: Volume, gal Density, Ib/gal Weight, lb Unreduced material 1.00 7.74 7,74 Reducing thinner 0.20 7.20 W where (reducing thinner), weight = volume x density, or - 0.20 X 7.20= 1.441b:' , - (2) The density of the reduced material is obtained by adding the volume and weight of each component, and dividing the total weight by the total volume: Volume, gal Unreduced material Reducing thinner 1.00 0.20 1.20 9-.18 where density of reduced paint = = 7.65 Ib/gal. 5.6.2.2 Formula Volume Solids of Reduced /`unit Knowing Percent Reduction and Unreduced Volume Solids Using the information from the previous example and assuming an unreduced volume solids,of 50 % and a volume reduction of 20 % thiniier,. the reduced formula volume solids content {S,,) is calculated as follows: Volume, gal Unreduced material Reducing thinner 1.00 0,20 1.20 0.50 where formula volume solids,jeduced = = 0.42 gal, or S,, = 42.0 %. 6. Precision and Bias 6.1 No statement is made about either the precision or bias of this practice for calculating formulation physical constants since the results are obtained strictly by mathemat ical calculations and will be related to the accuracy of the data used and conformance to the prescribed calculations. 6.2 A bias toward slightly smaller volumes and highu densities may result from non-ideal solution behavior (see 1.3, (2)). 7. Keywords 7.1 density; formulation; physical constants; solids con tent; volatile organic compound, (VOC) 1000 DUP050298178 ased on th. 'ing Perce,;'1 tie In 5.1.[ 1 ler having i Weigii, lb # D 5201 roe American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible-technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend If you fool that your comments have not received a fair hearing you should make your views known to tha ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 79703. '! Jbtained by, onent, ana t ced Paint, me Solids" ample and d a volutneji la volume olids, gal 0.50 0.00 0.50 t.42 gal, or ecision oi l physical nathematicy of the ilations. nd higher, avior (see )Iids con- 1001 DUP05 0298179 Designation: E 97 - 82 (Reapproved 1987) Standard Test Method for Directional Reflectance Factory 45-deg 0-deg, of Opaque Specimens by Broad-Band Filter Reflectometry1 This standard is issued under the fixed designation E 97; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, rise year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<s) indicates an editorial change since the last revision or reapproval. This method has been approvedfor use by agencies oftheDepartment ofDefense andfor listing in theDoD Index ofSpecifications and Standards. 1. Scope 1.1 This method covers the determination of the 45-deg, 0-deg directional reflectance factor ofnonfluorescent opaque specimens by means of filter photometers. To obtain similar results from spectrophotometers, see Method E 308. Nz{' l^=The values stated in inch-pound units are to be regarded as the standard. N|}' 2--This method has been developed for determining (1) the daylight luminous reflectance factor of paint, opaque white porcelain enamels, and ceramic whitewares; and (2) the blue-light reflectance factor (sometimes called "brightness") of uncolored papers and pulps in sheet form. The method may also be used for determining the reflectance factor of other opaque specimens. N~' 3--The blue-light reflectance factor of paper provides a measure of freedom from yellowness such as results in pulp and paper from the presence of lignin and other so-called impurities left by incomplete bleaching. N' 4--Blue-light reflectance factor by this method differs slightly, both spectrally and geometrically from the TAPPI Stahdards T 217 and T 452. The TAPPI methods are considered to be standard for the pulp and paper industry when brightness measurements are to be made. 1.2 This standard may involve hazardous materials, oper ations, and equipment. This standard does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofwhoever uses this standard to consult and establish appropriate safety and health practices and deter mine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: C 347 Test Method for Reflectance, Reflectivity, and Coefficient of Scatter of White Porcelain Enamels2 D 523 Test Method for Specular Gloss3 D 585 Method for Sampling and Accepting a Single Lot of Paper, Paperboard, Fiberboard, or Related Product4 D823 Test Methods for Producing Filins of Uniform Thickness of Paint, Varnish, and Related Products on Test Panels3 'This method is under the jurisdiction of ASTM Committee E-12 on Appearance of Materials and is the direct responsibility of Subcommittee E12.03 on Geometric Practices. Current edition approved Oct 29, 1982. Published December 1982. Originally published as E 97 - 53 T. Last previous edition E 97 - 77. 2 Annual Book ofASTM Standards, Vol 02.05. 3 Annual Book ofASTM Standards, Vol 06.01. 4 Annual Book ofASTM Standards, Vol 15.09. E 179 Practice for Selection of Geometric Conditions for Measurement of Reflectance and Transmission Proper ties of Materials5 E 284 Terminology Relating to Appearance of Materials5 E 308 Method for Computing the Colors of Objects By Using the CIE System5 2.2 TAPPI Standards:6 T 217 Brightness of Pulp T 452 Brightness of Paper and Paper Board 3. Significance-and Use 3.1 Measurements of reflectance factor provide a measure of the amount of incident radiation reflecting diffusely under the geometric conditions of this method. High values indi cate low absorption. When the response of the detector conforms to the sensitivity of the average human eye (Y-tristimulus filter), the result is designated luminous reflec tance. For near white specimens, the reflectance value for blue light (Z-tristimulus filter), provides a relative index of freedom from yellowness for a particular type of material. 3.2 This method is frequently used to evaluate near-white, diffusely reflecting materials such as paint, paper, and powders. 4. Terminology 4.1 reflectancefactor--ratio of flux reflected from a spec: imen to the luminous flux reflected from a standard surface, under the same geometric conditions of measurement. Unless otherwise indicated, the-standard surface is assumed to be a perfect reflecting diffuser. If some real surface is used, the quantity measured is called "relative reflectance factor." 4.2 daylight 45-deg, 0-deg luminous directional reflectance factor--the ratio of the luminous flux from a specimen illuminated at an angle of 45 deg and viewed perpendicularly by the equivalent of CIE standard source C and the 1931 CIE standard observer, to the luminous flux from the perfect reflecting diffuser, similarly illuminated and viewed (see Definitions E 284). N' 5--The combination of illumination at 45-deg and viewing at 0-deg (perpendicularly), designated 45/0, or the converse designated 0/45, has been selected as being representative of average conditions of illuminating and viewing. This reflectance factor determines which of 5 Annual Book ofASTM Standards, Vol 14.02. 4 Available from Technical Association of the Pulp and Paper Industry, P.O. Box 105113 Atlanta, GA 30348. 1002 w speci1 Sch th^ Appt 15.1 T Wil q desf nee faj 'he ap| ^.l.f 1 atpr ah Ition* f adafri, imetioii |N' f 5oran| [the Ctf. hinositi 5.1.1.1 pr--Th nsmii equi' ' ndayc ' stai .5,1,2 iithinjdf l fret*,,-ctivefc ad cenf:. f N' ay bss up nbediri. dorm if"' liven instil. specif!;;, ref" . Stamjr. 6-1 /i ace is is t lions E 45-deg i|l h TThe n| uremrf Available fe D1201. 1 DUP050298180 .specimens will appear lighter when viewed m daylight at an angle at ph the observation of highlights is avoided. '.3 blue-light 45-deg, 0-deg directional reflectance fac-the ratio of the light flux from the specimen illuminated i angle of 45 deg by CIE standard source C, and viewed !-endicularly by a receptor whose response is equivalent to z-function of the CIE standard observer, to the light flux i the perfect reflecting diffuser similarly illuminated and Ived (see Definitions E 284). ' '' 6--CIE standard sources and functions are defined in Method 8. 'Apparatus *.l The apparatus shall consist of a reflectometer, either al or photoelectric type, having source, filter, receptor, d design characteristics such that it will measure reflec:e factors accurately to within 1.0 % of full-scale reading. : apparatus shall have the following characteristics: 8.1.1 Spectral Characteristics: '.,1.1.1 For Measurement of Daylight Luminous Rejlecfe Factor--The spectral energy distribution of the iilumipr and the spectral sensitivity of the receptor, in combi nin', shall provide the equivalent of illumination by CIE udard source C and observation by the luminosity (y) fiction of the 1931 CIE standard observer. N' 7---Spectra! characteristics based on CIE standard illuminant or any other CIE daylight standard illuminant, or on the y function ..the CIE 1964 supplementary standard observer (which is not the inosity function) may be used as an alternative. -5,1.1.2 For Measurement of Blue-Light Reflectance Fac- r--The product of spectral energy of source, spectral nsmission of filters, and spectral response of receptor shall equivalent to the product of the z-function of the CIE ndard observer multiplied by the energy distribution of ; standard source C. 5.1.2 Geometric Characteristics--Illumination shall be thin 4 deg of, and centered about, a single direction of 45 g from the perpendicular to the test surface. It shall be ectively nonpolarized. Viewing shall be within 15 deg of, d centered about, the perpendicular. j' - ; |;'N' 8--Any instrument that meets these apparatus specifications Jay be used. Instruments should also meet the precision requirements Sscribed in Section 11. In general, commercial instruments do not nform exactly to the apparatus requirements. The suitability of a ven instrument depends in large measure on the spectral selectivity of 'e specimens being measured, and on the availability of standards of rtnilar reflectance and spectral character.7 8 Standards . 6.1 Primary Standard--The primary standard for reflec* nee is the perfect reflecting diffuser as described in Definiions E 284. It is assigned a value of 100 for the conditions of ,5-deg illumination and perpendicular view. 6.2 Secondary Standards8--Porcelain-enameled metal plaques, or other materials known to be reasonably perma nent in reflectance and uniform over the surface, may be calibrated and used as secondary reflectance standards. 7. Preparation of Test Specimens 7.1 Paint--Unless otherwise specified, prepare panels for the determination of reflectance factor by applying the paint to a suitable flat background with a doctor blade in accord ance with Test Methods D 823. Use sufficient thickness so that additional coats produce no measurable change in reflectance factor. Allow 72 h for the.paint to dry. It is recommended that 60-deg gloss as described in Test Method D 523 and unusual surface structure be noted. 7.2 Porcelain Enamel--Laboratory-prepared specimens, articles of commerce, or sections cut from articles of commerce may be tested. The area to be tested shall be flat and reasonably free of surface defects. Laboratory specimens shall be at least 60 by 90 mm (2 Vi by 3V2 in.) in size; however, specimens 100. by 100 mm (4 by 4 in.) are preferred. N' 9--The method ofpreparation of the specimen, such as weight of application or firing treatment, may affect the reflectance factor but is not a part of this test method- however, each manufacturer should investigate the effect of such variables on the reflectance factor of his products (see Test Method C 347). 7.3 Paper--Sample in accordance with Test Methods D 585. Handle the test specimen carefully to avoid soiling, and take care not to touch the areas to be tested. The test specimen shall consist of a pad of sheets sufficiently thick that doubling the number of sheets causes no measurable change in reflectance factor. 7.4 Other Materials--Prepare test specimens of materials other than those listed in 7.2 and 7.3 in accordance with accepted practice,, and record the method of preparation in the report. N' 10--All high-reflectance diffusely reflecting materials are somewhat translucent since most of their reflectance is due. to internal scattering. Roughly 95 % of the incident light is transmitted through the surface, and partially absorbed. What is not absorbed is multiply scattered back to the surface, at a point different from the point of incidence, where it is retransmitted as reflected light. The maximum distance between the points of incidence and exitance is primarily a function of the extinction coefficient of the material. For materials such as most white paints and porcelain enamels, the extinction coefficient is large, and the maximum distance of travel is small, and errors due to this internal travel' may be small enough to be neglected. Other high-reflectance materials, such as opal glass and white plastics, may have smaller extinction coefficients, and the maximum distance of internal travel may be large enough (several millimetres is not un common) that significant light losses can occur unless the reflectometer has been designed to eliminate such losses. The maximum errors occur in measurements of reflection factor when comparing sample and standard of markedly different extinction coefficients. See NBS Tech nical Note 594-12 (Oct. 1976) fora detailed discussion of such losses. 7 The names and addresses of manufacturers producing instruments for the ' easurement of reflectance are listed in Optica! Industry and Systems Directory, variable from Optical Publishing Co., Inc., P.O. Box 1146, Pittsfield, Mass. 1201. 8 Secondary standards of porcelain enamel may be obtained from the Hunter Associates Laboratory, Inc., ! 1495 Sunset Hills Rd., Reston, Va. 22090, or the Gardner Laboratory Division of Pacific Scientific, P.O. Box 5728, Bethesda, Md. 20014. Other sources of standards may be obtained by writing to ASTM Headquarters. 1003 DUP050298181 E 97 8.Procedure 8.1 Operate the reflectometer in accordance with the instructions supplied by the manufacturer, including line voltage, warm-up time, and adjustment of the scale. 8.2 Use a standard having a reflectance factor close to that of the test specimen or, if several specimens having a small range of reflectance factor values are being tested, use at least two standards, preferably at the extremes of the range being measured. Use a green filter for luminous reflectance factor; a blue filter for blue-light reflectance factor of paper or other materials; and, when specified, other filters for reflectance factor for other kinds of light, such as an amber filter for amber-light reflectance factor, etc. N' 11--In general, instrumental errors are related to the differ ences in reflectance factors and spectral characteristics between specimen and standard. For greatest accuracy, standards close in reflectance factor and similar in spectral characteristics to the specimens should be used. The same area of standard should be measured as that used for its calibration. 8.3 Obtain the instrument readings for the standards and then for the specimens, in turn; read the specimens in reverse order, and finally read the standards again. 8.3.1 Paper Specimens--Make readings with the blue filter on at least five separate sheets, and equal numbers of readings parallel to and at right angles to the machine direction of the paper on both sides of the sheets. 8.3.2 Porcelain-Enameled Specimens--Make reflectance factor readings with the green filter on an area not less than that ofa circle 70 mm (2% in.) in diameter. A determination shall comprise a sufficient number of readings so that the average of successive determinations can be reproduced with a difference between the highest and lowest determinations, not exceeding 0.5 % on the scale for which the perfect reflecting diffuser is assigned a value of 100 (see 6.1). Instruments covering areas smaller that that prescribed may be used, provided a sufficient number of well-distributed readings is taken so that the average reflectance factor is determined within the spread prescribed for repeated deter minations on a given specimen.9 9.Calculation 9.1 Calculate the mean value for the readings on each standard and specimen. 9.2 Calculate the reflectance factor of each specimen according to the directions of the instrument manufacturer. Apply corrections for scale nonlinearity, if available. In the absence of more explicit instructions, calculate the specimen reflectance factor as follows; U = (RJb) where: R = reflectance factor of the specimen for the filter used c = mean instrument reading for the specimen, b = mean instrument reading for the standard used, and Rs = assigned reflectance factor of the standard for the filter used. N' 12--The scale linearity of an instrument may be checked by reading the reflectance factors of a series of ten or more nonselective standards ranging from 85 to 0.5 %.s 10. Report 10.1 Report values of reflectance factor in percent relative to the perfect reflecting diffuser as 100 (as defined by U.Si National Bureau of Standards). The result is described as "45-deg, 0-deg directional reflectance factor." When the green filter is used, the words "daylight luminous" shall be inserted before "directional." When the blue or amber filters are used, the phase "for blue light" or "for amber light," respectively, shall be added after "reflectance factor." Report reflectance factor values to the nearest 0.1 %. For paper' specimens, report values for the wire and felt sides separately.'1 10.2 Describe or otherwise identify the method of pre paring laboratory specimens. 10.3 Identify the reflectometer used by the manufacturer's name, the model, and the serial number. \ 11. Precision H.l Precision (Repeatability and Reproducibilityj^'R.epeatability is the deviation from mean experienced when measuring a single specimen on a single instrument. Note' ^ that with many samples measured, excessive nonuniformity' ; by area, or by method of presentation to the instrument, is' the chief factor limiting repeatability. Reproducibility is the deviation from mean experienced between different instru ments employing calibrated standards of nearly the same reflectance factor. Refer to Table 1. mi TABLE 1 Precision Data4 N' --All values refer to standard deviations. Measurement Reproducibility Repeatability Directional blue reflectance V Reflectance factor 1 Reflectance factor 0.4 0.7 o.a 0.2 not available not available A TAPPI Collaborative Reference Program for Paper; NBS; Reports 1 to 10 and 28 to 33; MCCA Collaborative Reference Program for Color and Appearance. h v2; Bl The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are express/y advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and it not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend, if you feel that your comments have not received a fair hearing you should make your weivs known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. feppef, Sn Stiff 1004 DUP0502981 82 Designation: E 259 - 91 Pecimert r used, d, and the filter".1 iecked by nselectivc Standard Practice for Preparation of Pressed Powder White Reflectance Factor Transfer Standards for Hemispherical Geometry1 This standard is issued under the fixed designation E 259; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year oflast revision, A number In parentheses indicates the year oflast reapproval. A superscript epsilon (if indicates an editorial change since the last revision or reapproval. INTRODUCTION relative by U.S.' ribed as hen the. shall be er filters r light," ' Repon r paper' >arately. of pre- icturer's vf--Re1 when t. Note formity nent, is y is the instrue same ^_____ )te >le lo 10 and ance. The internationally accepted standard of reflectance is the perfect reflecting diffuser. This ideal reflecting surface reflects 100 % of the radiant power incident ori it such that the radiance is the same for all directions within the hemisphere of solid angles. No physical realization of this standard exists. Optical properties of standards prepared from pressed plaqties of magnesium carbonate (MgC03), barium sulfate (BaS04), or polytetrafluoroethylene (PTFE) can approximate those ofthis ideal standard. For further information see CIE Publication No. 46 (l).2 The principal use of a white reflectance factor standard is to transfer an absolute scale of reflectance to a more durable material or from one instrument td another. In theory, this transfer, done from first principles, should-be quite easy. In practice, values are likely to be required for parameters that are unknown, proprietary; or require a highly sophisticated level of skill. Some, but not all, of those parameters are discussed in this practice. Scope 1.1 This practice covers procedures for preparing pressed iwder transfer standards of reflectance factor. .These stan ds can be used in the near-ultraviolet, visible and near ed region of the spectrum. Procedures for calibrating reflectance factor of materials on an absolute basis are intained in CIE Publication No. 44 (2). Pressed powder .tidards are used as transfer standards for such calibrations tuse they have a high reflectance factor wfhichis nearly <nstant with wavelength and because the distribution of fleeted flux resembles that from the perfect reflecting iffuser. 1.2 This standard does not purport to address all of the ifety problems, if any, associated with its use. It is the isponsibility ofthe user of this standard to establish appro bate safety and health practices and determine the applica|/hy ofregulatory limitations prior to use. 1.3 The values stated in SI units are to be regarded as the Ijkndard. The values in parentheses are for information only. I Referenced Documents 2.1 ASTM Standards: s E 284 Terminology of Appearance3 D1457 Specification for Polytetrafluoroethylene (PTFE). Molding and Extrusion Materials4 1 This practice is under the jurisdiction of ASTM Comroittee E-12 on ppearanee of Materials and is the direct responsibility of Subcommittee E12.02 it Spectrophotometry and Colorimetry. Current edition approved Aug, 15. 1991. Published October 1991. Originally ublisbed as E 259 - 65. Last previous edition E 259 - 66 {1987). 2 The boldface numbers in parentheses refer to the list of references at the end f this practice. 3 Annual Book ofASTM Standards, Vol 14.02. 4 Annual Book ofASTM Standards, Vol 08.01. D4894 Specification for Polytetrafluoroethylene (PTFE) Granular Molding and Ram Extrusion Materials5 3. Terminology 3.1 Definitions--All terms used in this practice are consis tent with Terminology E 284. The following three definitions are particularly important to this practice: 3.1.1 reflectance--the ratio of the flux reflected from a specimen to the flux incident on the specimen. 3.1.2 perfect reflecting diffuser--ideal reflecting surface that would neither absorb nor transmit light, but would reflect diffusely, with the radiance of the reflecting surface the same ,for all reflecting angles, regardless of the angular distribution of the incident light. 3.1.3 reflectancefactor--the ratio of flux reflected from a specimen to the flux reflected from a standard surface, under the same geometric conditions of measurement. Unless otherwise indicated, the standard surface is assumed to be the perfect reflecting diffuser. 4. Summary of Practice 4.1 Procedures are given for the preparation of white reference standards of diffuse reflectance factor. The recom mended materials are white powders that are pressed into plaques. These plaques provide close approximations to the optical properties of the perfect reflecting diffuser, and may be used to transfer a scale of absolute reflectance to another material or to an instrument. 4.2 Previous editions of this practice included guidelines for the preparation of standards from magnesium oxide smoke. Preparation of this type of standard is no longer recommended. The ease of preparation, physical ruggedness. 5 Annual Book ofASTM Standards, Vol 08.03. 1005 DUP050298183 l> E 259 and photometric stability of pressed powder plaques make them far superior to smoked magnesium oxide plaques as reflectance factor standards. 5. Significance and Use 5.1 All commercial reflectometers measure relative reflec tance. The instrument reading is the reflectance factor, the ratio of the light reflected from a reference specimen to that reflected from a test specimen. That ratio is dependent on specific instrument parameters. 5.2 National standardizing laboratories and some research laboratories measure reflectance on instruments calibrated from basic principles, thereby establishing a scale of absolute reflectance as described in CIE Publication No. 44 (2). These measurements are sufficiently difficult that they are usually , left to laboratories that specialize in them. 5.3 A standard that has been measured on an absolute, scale could be used to transfer that scale to a reflectometer. While such procedures exist, the constraints placed on the mechanical properties restrict the suitability of some of the optical properties, especially those properties related to the geometric distribution ofthe reflected light Thus, reflectance factor standards which are sufficiently rugged and cleanable to use as permanent transfer standards depart considerably from the perfect diffuser in the geometric distribution of reflected radiance. 5.4 The geometric distribution of reflected radiance from a pressed powder plaque is sufficiently diffuse so that such a standard can provide a dependable calibration of a direc tional-hemispherical reflectometer. Although pressed powder standards are subject to contamination and breakage, the directional-hemispherical reflectance factor of pressed powder standards can be sufficiently reproducible from specimen to specimen made from a given lot ofpowder, so as to allow one to assign absolute reflectance factor values to all the ppwder in a lot. 5.5 This practice describes how to prepare white reflec tance factor standards from a powder in a' manner that allows a standardizing laboratory to assign the absolute scale of reflectance to the powder. 6. Apparatus .6.1 The basic apparatus for producing a pressed powder standard includes a powder press, powder containers and a balance. There are presently two commercial suppliers of powder presses.6 The press and receptacles can also be made in a local machine shop. A suggested configuration is shown in Fig. 1. The optical surface of the plaque should be pressed against a surface of ground glass or polyfmethyl methacrylate) to provide a matte finish on the pressed plaque. Powder receptacles should be at least 5 mm deep for BaS04 and at least 10 mm deep for PTFE. HUNGER COLLAR RECEPTACLE N' --The collar and receptacle should be securely held in place before pressing the powder. FIG. 1 Example Powder Press highest purity. It should be specially refined for optical and spectroscopic use (3).7 8.2 Polytelrqfluorpethylene--the PTFE (4)8-9-10 should also be specially refined for optical and spectroscopic use but some commercial grades have been found, to be acceptable substitutes. There is currently no commercial source for small quantities of optical grade PTFE .powder. Large quantities (drums) of commercial grade PTFE can be ob tained from the manufacturers. 9. Procedure 9.1 All powdered reflectance standards should be stored m tightly capped glass containers. If the powder is purchased m plastic containers it should be.transferred to a glass container' as sooii as possible. Before using the powder, it should be* placed in a glass blender equipped with stainless-steel or PTKE-coated blades and pulverized to a uniform consis tency. The quantity of powder to be used should be transferred with stainless steel or PTFE-coated spoons, The wholeoperation should be performed in a draft-free location, away from sources of small particulate contamination, filters, sweaters, windows, ovens, etc. All measurements (weight, height, width, depth; volume, area, etc.) should be performed with adequate precision to ensure that the final density is within 5 % of the specified value. The'iftost . reproducible standards are made by pressing the powder to a specific density. Thus, the mass of the powder to be used should be determined from the volume of the receptacle. 9.2 Barium Sulfate--BaS04 should be pressed to a den sity of 2000 kg/m3 (2.0 gm/cm3) and a thickness of at least 5 mm. Several specimens should be pressed in succession. Matched pairs should be selected to be representative of the contents of the bottle ofpowder. The pressed plaques should be kept in a covered desiccator when not in use. Some suppliers of BaS04 parovide calibration values with each 8. Reagents and Materials 8.1 Barium Sulfate--the barium sulfate should be of the 6 Powder press conforming to ISO 2469 and DIN 5033 is available from Carl Zeiss Canada, Ltd., 45 Vaileybrook Drive, Don Mills, Ontario M3B-2S6, Canada, Part Number 505866; and Technidyne Corporation, 100 Quality Avenue, New Albany, IN 47150-2272, Part Number 176601. 7 One such material, Kodak "White Reflectance Standard 6091, available from Eastman Kodak Company, Laboratory and Research Products Division, Rochester, NY 14650, has been found suitable for this purpose. 8PTFE-M-12, available from Daikin Industries, Ltd., l-l Nishihitotsuya Yodogawa, Siesakusho, Setto-Shi, Osaka, Japan, has been found suitable. 9 TEFLONTM 7A, available from 6.T. DuPont de Nemours & Co., Inc., Barley Mill Plaza, Wilmington, DE 19880, has been found suitable. ,0AlgoFIon F5, available from AUSIMONT USA, Inc., CN 1838-T. Morristown, NJ 07960, has been found suitable. 1006 TABt; ' || . A Densitj :. B Accifre fettle.qf ; Jlferen^e ieferenfcef. he 6/idi * leflectkr;. 9.3 Af. ensityj d' last i;0 $ iiaximutf*' prepared tepreseptg'' pressed d). DUP0502981 84  E 259 < { ' IR TABLE 1 $`7Diffuse Reflectance Factor of Eastman White Reflectance Standard'1 Pressed BaS04 Powder4 Wavelength, nm Reflectance Factor 300 u 350 l 400 450 ! 500 550 S; 600 650 700 : 750 aoo ' 850 ii '900 f- 950 f 1000 0.968 0.979 0.987 0.991 . 0.991 0.992 0.992 0.992 0.992 0.992 0.992 0.991 0.990 0.988 0.986 * Density = 2000 kg/m3 and thickness = 5 mm. TABLE 3 Average and Standard Deviation of S/Diffuse Reflectance Factors of 17 PTFE Plaquas Prepared by 9 Laboratories Wavelength, nm Reflectance Factor Average* Standard Deviation8 300 350 400 500 600 700 800 1000 0.9792 0.9863 0.99T1 0.9919 0.9915 0.9914 0.9912 0.9910 0.0063 0.0021 o.oai8 0.0020 0.0023 0.0023 0.0024 (T.0024 A Average Density 926.2 kg/m3. B Standard Deviation = 85.7 kg/m3. rul TABLE 2 6/Diffuse Reflectance Factor of Pressed PTFE tiki * Powder4 but tble for age ob- Hbi' hit iter K1 or Wavelength, nm 300 350 400 450 500 550 600 650 700 750 800 850 900 950 1000 Reflectance Factor3 0.984- 0.990 0.993 0.993 0.994 0.994 0.994 0.994 0.994 0.994 0.894 Qi994 0.994 0.994 0.994 v. 1 Density = 100Q kg/ma and thickness > 5 mm. be * Accurate to i=0.QQ2.' 'he m. te|ttle of powder, other suppliers provide only 3 or 4 quality m iJerence checks and a reference to published values of its reference standards prepared from the powder. Table 1 gives x ge 6/diffuse reflectance factor values for Eastman White oat e&j oa >ed : leflectance Standard.6 [9.3 Pofytetrafluorethylene--PTFE should be pressed to a Snsity of 1000 kg/m3 (1.0 gm/cm3) and a thickness of at last 10 mm. The spectral reflectance reaches a broad 3n- tjaximum near this density. Several specimens should be t5 lepared in succession. Matched pairs are selected to be >n. Ipresentative of the contents of the bottle of powder. The he iessed plaques should be kept in a desiccator when not in ild ne ch use. PTFE can be very sensitive to particulate contamination and electro-statically attracts airborne particles. Such con tamination can make the material slightly fluorescent and reduce its reflectance in (he ultraviolet spectral region. Table 2 lists the 6/diffuse reflectance factor values for PTFE as determined by the National Institute of Standards and Technology (NIST). 10. Precision and Bias 10.1 The National Institute of Standards and Technology and the Inter-Society Color Council Project Committee 22, Materials for Instrument Calibration, have carried out col laborative tests to determine the precision and bias of the preparation of PTFE reflectance factor standards (5). The standard deviation of three determinations of the reflectance factor of PTFE by the NIST ranged from 0.0002 to 0.0008 over the spectral range 300 to 1000 nm. The measured reflectances of PTFE from two manufacturers exhibited differences of from --0.002 to +0.004 over the same range with the largest differences near the ends of the.range and a constant measurement uncertainty of 0.005. From the 9 laboratories participating in the round-robin experiment, 17 specimens were returned. The results are shown in Table 3 for the wavelength range 300 to 1000 nm. 10.2 CIE Publication Number 46 (6) cites literature references on the reproducibility of BaS04 pressings that range from 0.05 % to 1.0 % with the most common value in the range about 0.2 %. This puts the reporducibility of the plaque preparation near the level of the reproducibility of the international standardizing laboratories' ability to charac terize the absolute reflectance of the material. 301 0i lya ley 1 1007 DUP050298185 E 259 REFERENCES (1) Publication CIE No. 46--A Review ofPublications on Properties and Reflection Values ofMaterial Reflection Standards, available from U.S. National Committee CIE (International Commission on Illumination), % Director of Marketing, OEM Division, North American Philips Lighting Corp., Philips Square, CN6800, Somerset, NJ 08873. (2) Publication CIE No. 44--Absolute Methods for Reflection Mea surements. available from U.S. National Committee CIE (Interna tional Commission on Illumination), % Director of Marketing, OEM Division, North American Philips Lighting Cotp., Philips Square, CN6800, Somerset, NJ 08873. (3) Gram, F., and Wightman, T. E., "Absolute Reflectance of Eastman White Reflectance Standard", Applied Optics, Vol 16, 1977, pp. 2775-2776. (4) Weidner, V. R., and Hsia, J. J., "Reflection Properties of Pressed Polytetrafluoroethylene Powder," J. Opt. Soc. Am., Vol 71, i gg j pp 856-861. (5) Weidner, V. R,, Hsia, J. J., and Adams, B., "Laboratory Intercomparision Study of Pressed Polytetrafluoroethylene Powder Reflectance Standards," Applied Optics, Vol 24, 1985 nD 2225-2230. (6) Publication CIE No. 38--Radiometric and Photometric Character istics ofMaterials and Their Measurement, available from U.S. National Committee CIE (International Commission on Illumina tion), % Director of Marketing, OEM Division, North American Philips Lighting Corp., Philips Square, CN6800, Somerset, NJ 08873. The American Society tor Testing end Materials takes no position respecting Me validity ofany patent rigWs asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that,determination of the validity of any such patent rights, and tha risk of infringement of such rights, are entirely their own responsibility. This standardis subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited eitherforrevision ofthis standardor foradditionalstandards and Should be addressed to ASTM Headquarters. Your comments v/llt receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee oh 'Standards, 1916 Race St., Philadelphia, PA 19103. 1008 DUP050298186 Designation: E 430 - 91 Standard Test Methods for oa Measurement of Gloss of High-Gloss Surfaces by *1. Goniophotometry1 ten dcr 'I rp This standard is issued under the fixed designation E430; the number immediately following the designation indicates the year of original adoption or, in the case ofrevision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {) indicates an editorial change since the last revision or reapproval. ' Cr- f.s.. jpcope 03- |l These test methods cover the measurement of the :tion characteristics responsible for the glossy appear- NJ: j of high-gloss surfaces. Two test methods, A and B, are vided for evaluating such surface characteristics at jfpular angles of 30 and 20, respectively. These test (hods are not suitable for diffuse finish surfaces nor do measure color, another appearance attribute. ;.2 As originally developed by Tingle and others (see Refs ad 2),12 the test methods were applied only to bright Itals. Recently they have been applied to high-gloss autoItive finishes and other nonmetallic surfaces. !| Referenced Documents . 11 ASTM Standards: j^D 523 Test Method for Specular Gloss3 >2457 Test Method for Specular Gloss of Plastic Films and Solid Plastics4 'ft 171 Specification for Standard Atmospheres for Condi tioning and Testing Materials5 i 179 Practice for Selection of Geometric Conditions for Measurement of Reflectance and Transmission Proper ties of Materials6 1 284 Terminology of Appearance6 308 Test, Method for Computing the Colors of Objects , by Using the CIE System6 1347 Test Method for Color and Color-Difference Measurement of Object-Color Specimens by Tristimulus (Filler) Colormetry6 Terminology 13.1 Definitions: J3.1.1 Reflectance and Related Terms: 13.1.1.1 reflectance, p, n--ratio of the reflected radiant or minous flux to the incident flux in the given conditions. 1284) |(7,I Discussion--The term reflectance is often used in a literal sense or as an abbreviation for reflectance factor. 1 These test methods are under the jurisdiction of ASTM Committee E-12 on Ipearance of Materials and are the direct responsibility ofSubcommittee E 12.03 1 Geometry. I Current edition approved Aug. 15, 1991. Published November 1991. Originally jfblished as E 430 -71. Last previous edition E 430 -78(1983). r2 The boldface numbers in parentheses refer to the list of references at the end |this method. Annual Book ofASTM Standards* Vo! 06.01. 4 Annual Book ofASTM Standards, Vol 08.02. |s Annual Book ofASTM Standards, Vol 15.09. 6 Annual Book ofASTM Standards, Vol 14.02. Such usage is not assumed in this' method. The definition may require that the term be modified by adjectives denoting the spectral and geometric conditions of measurement. 3.1.1.2 reflectancefactor, R, n--ratio of the flux reflected from the specimen to the flux reflected from the perfect reflecting diffuser under the same spectral and geometric conditions of measurement. (E 284) 3.1.1.3 gloss reflectance factor, n--ratio of the specularly reflected part of the, (whole) flux reflected from the specimen to the flux reflected from a specified gloss standard under the same geometric and spectral conditions of mea surement. (1) Discussion--The gloss standard may be a black glass or a mirror, and may be assigned one ofa variety of scale values Gs as specified. (E 284) 3.1.2 Gloss and Types ofGloss: 3.1.2.1 gloss, n--angular selectivity of reflected light, responsible for the degree to which reflected highlights or images of objects may be seen as superimposed on a surface. (E 284) (1) Discussion--Gloss is responsible for the object's glossy appearance, not for an observer's perception of the appear ance. At least six types or characteristics of gloss may be observed depending upon the character of the surface and the spatial distribution of the reflected light (3). 3.1.2.2 specular gloss, n--ratio of flux reflected in specular direction to incident flux for a specified angle of incidence and source and receptor angular apertures. (E 284) 3.1.2.3 distinctness-of-image gloss, n--aspect of gloss characterized by the sharpness of images of objects produced by reflection at a surface. (E 284) 3.1.2.4 sheen, n--the specular gloss at a large angle of incidence for an otherwise matte specimen. (The usual angle for measurement is 85.) (E 284) 3.1.3 Terms Relating to Surface Characteristics: 3.1.3.1 directionality, n--perceived, the degree to which the appearance of a surface changes as the surface is rotated in its own plane, under fixed conditions of illumination and .viewing. (E 284) 3.1.3.2 texture, n--the visible surface structure depending on the size and organization of small constituent parts of a material; typically, the surface structure of a woven fabric. (E 284) 3.1.4 Other Terms: 3.1.4.1 aperture angle, 2h n--angle subtended at a point on a specimen by the maximum dimension of the illumi nator or receiver, within which the flux in a directional beam is contained. (1) Discussion--In optics, the symbol k is used for the 1009 DUP050298187 E 430 half angle; hence the recommended symbol here is 2h (E 284) 3.1.4.2 goniopkotometer, n--instrument that measures flux as a function of angles of illumination or observation. (E284) 3.2 Terms Specific to This Test Method: 3.2.1 Terms Relating to Reflection Haze: 3.2.1.1 reflection haze, H, n--for a specified specular angle, ratio of flux reflected at a specified angle (or angles) from the specular direction to the flux similarly reflected at the specular angle by a specified gloss standard. (1) Discussion--Modifiers may. be used to specify the angles at which the haze is measured (for example, 2" or 5); whether H or a logarithmic form is to he stated; or whether H is to be compensated for the luminance of the specimen by multiplication by I'sp-cmcn/T',,, where n denotes the reference white; or any combination of these. 3.2.2 Terms Relating to Metallic Reflection: 3.2.2.1 metallic brightness, n--freedom of a metal surface from diffuse haze or texture. 3.2.3 Terms Relating to Specimen Directionality: 3.2.3.1 `with-machine' direction, n--the axis of a spec imen that is parallel to the direction of mill rolling or extrusion, or other surface-finish texture. 3.2.3.2 'across-machine' direction, n--the perpendicular to `with-machine' direction. 3.3 Other appearance terms and definitions in Termi nology E 284 are applicable to this test method. 4. Summary of Test Method 4.1 Several geometrically different measures of light re flected by a surface are proposed for use in describing its gloss appearance. In Test Method A, gloss reflectance factor is measured at 30 to the specimen normal using narrow illuminator and receiver aperture angles (0.5 wide max imum). Distinctness-of-image gloss is measured at 29.7 or 30.3 or both. Narrow-angle (2) reflection haze is measured at 28 or 32or both, and wide-angle (5) reflection haze at 25 or 35 or both. The ratio of reflectance factors for 28 or 32 or both, perpendicular and parallel to the machine direction of the specimen, is computed as a measure of directionality. In Method B, specular gloss is measured at 20 according to Test Method D 523, and narrow-angle reflection haze is measured at 18.1 and 21.9.5 5. Significance and Use 5.1 The gloss of metallic finishes is important commer cially on metals for automotive, architectural, and other uses where these metals undergo special finishing processes to produce the appearances desired. It is important for the end-products which use such finished metals that parts placed together have the same glossy appearance. 5.2 It is also important that automotive finishes and other high-gloss nonmetallic surfaces possess the desired finished appearance. The present method identifies by measurements important aspects of finishes. Those having identical sets of numbers normally have the same gloss characteristics. It usually requires more than one measurement to identify properly the glossy appearance of any finish (see Refs 3 and *) 6. Apparatus 6.1 The apparatus shall be either an abridg goniophotometer (see Figs. 1A and IB) or a goniophotometer (see Fig. 2) that can be set to the spec^ specular; off-specular, and aperture angles given in Tables Ph and IB. The abridged goniophotometer may have a fixe angle of incidence (for Test Method A, 30; for Test Methd B, 20) and specific fixed directions of view at which the f from the specimen is measured (see Tables 1A and I Bj 6.1.1 Geometric Conditions for Test Method A__' direction of incidence shall be 30 deg. The directions of shall be opposite the direction of incidence at 30 deg for. specular reflectance, 29.7 or 30.3 deg for distinctness of.i image comparisons, 28 or 32 deg for narrow-angle m4! j comparisons, and 25 or 35 deg for wide-angle haze comp; '* isons. The angular dimensions of the, mirror reflected i,r.t J., of the source slit in the plane of measurement and thd-4 angular dimensions of the receiver windows in this plane j ' measurement shall be as shown in Table 1A. N' 1--The conventional notation indicating positive angles fot I incident conditions and negative angles for viewing conditions has beeil used, thus far, to reduce confusion, in the remaining sections, tha'l negative notation is omitted, since only the viewing conditions are described. 6.1.2 Geometric Conditions for Test Method !i -i i.-l direction of incidence shall be 20 0.1. The direi ions . , view shall be opposite the direction of incidence, at 20 for specular gloss measurement and- at 18.1 and 2) ,l iri narrow-angle reflection haze measurement. The angular j dimensions ofthe specularly .reflected image ofthe soui c- s'.ti in the plane of measurement and the angular dimensions.of j the receiver windows in.this plane of measurement shall he j as shown in Table I B. 6.1.3 Spectral Conditions--The measurement shall be made with visible light to give results in accordance with theol CIE spectral luminous efficiency function F(X identical with y) in the CIE 1931 standard observer) and .CIE standard | iUuminant C (see Test Methods E 308 and E 1347), If S another iUuminant A, is used, this shall be specified m the j report. ; 6.1.4 Polarization--The incident flux shall be Uftpolu*-j ized and the receiver shatLbe insensitive to the state of| polarization of the reflected luminous flux. | 6.1.5 Clamp--For Test Method A, a rotatable clamp ofi the type shown in Fig. 3 may be used for flattening .t'ul j! positioning the specimen during measurement. 7. Standards 7.1 Three calibrated standards of good planarity shall be available in either a set of metals or a set of non metals, depending upon which type of surface is measured. 7.2 High-Gloss Standards: 7.2.1 High-Gloss Standard for Metals shall be of alu minum, evaporated onto glass and covered with a protective coating of silicon monoxide, and calibrated for specular gloss and distinctness-of-image gloss. 7.2.2 High-Gloss Standard for Nonmetals shall be of highly polished black glass with a refractive index of approx imately nD = 1.527, calibrated for specular gloss and reflection haze, and assigned a scale value of G$ = 89.4 for a 1010 i bfori,' mh iithfc DUP050298188 0! E 430 angle of 30 (Test Method A) or Gs = 89.2 for a far angle of 20" (Test Method B). E 2--To determine the scale value, calculate the first-surface ' j) reflectance (Test Method D 2457, Section 5.1) for nD = 1.567 ^.specular angle of interest; for 30" it is 5.0436 % and for 20" it is %. Assign this a;scale value of 100,(Test Method D 523, Section . eat the calculation for p = 1.527 and the same specular angle; lilt for 30" is 4.5069 % and for 20", 4.3769 %. The new scale value " is 100 X (4.5069/5.0436) = 89.4, and for 20", 100 X (4.3769/ : 89.2. (The latter value is also given in Test Method D 523.) Intermediate Standards: \ 1 Intermediate Standard for Metals shall be of either ium evaporated onto glass and covered with a protec coating of silicon monoxide, or of bright sheet alum with protective coating and calibrated for specular gland distinctness-of-image gloss. .2 Intermediate Standard for Nonmetals shall be of a ic material, such as porcelain enamel on steel, and `ted for specular gloss and distinctness-of-image gloss. 1 Diffuse Standards shall have a reflectance factor antially constant over the angular range of the instrut Care of Standards--It is essential that the standards. be kept clean and free of scratches as well as from contact with contaminating materials.,The cleaning method speci fied by the instrument manufacturer shall-be followed and the standards should be checked at-regular intervals against reference standards held in reserve. 8. Specimens 8.1 Specimens shall be obtained from test samples by selecting areas that are plane and representative of each sample being tested. Every specimen must be at least 2Va in. (70 mm) in the smallest dimension. Specimens may be larger so long a$ it is possible to insert, them and flatten them properly for measurement. 9. Preparation and Calibration of Apparatus 9.1 The instrument must be used in a clean dry area free of drafts. Standard laboratory conditions are recommended (see Section 2 of Specification E 171). Voltage regulation to 0.01 % must be incorporated in the instrument, or supplied separately. Follow manufacturer's recommendations for in strument warmup. 9.2 Calibration--Adjust the instrument to read the same 1011 DUP050298189 E 430 COtitEKSM LEMS SOURCE OBJECT LEH3 A RECEIVER RECEIVER OBJECT LESS generally coincides with the direction of travel of a sheet or film material through a processing machine. 10.4 Record the following quantities: - 10.4.1 For Test Method A, readings of(a) gloss reflectance factor (specular gloss), Rsj0 at 30"; (b> distinctness-of-image, gloss; (c) 2" reflection haze; H2\ and (d) 5" reflection haze, ff . The quantities in (b), (c), and (d) may be either giosj reflectance factors or values of H, which are their ratios ic the specular gloss reflectance factor recorded in (a). ! 10.4.2 For Test Method B, readings of (a) the 20 specular,; gloss, ,RSi20; (b) the reflection haze, //; and (c) the luminous reflectance, Y. ,, 10.5 Measure at least three areas of each specimen. 10.6 From these same areas, read 2-deg haze for the : "across-machirie direction," being careful to flatten the test surface andprient the specular beam in each case. 10.7 Take readings on the standards at the end of the series of observations to ensure that the instrument has: remained in calibration throughout the operation. FIG. IB Optical Diagram of the Apparatus for Method B gloss reflectance factor for the intensity of light reflected from the diffuse standard through the specular, distinctnessof-image, and haze apertures, Adjust the instrument to read values > of specular gloss and distinctness-of-image gloss assigned, the aluminum mirror if metal surfaces are being .measured; Or the black' gloss Standard if noruttetal surfaces are being measured. If the instrument does riot thenTead the appropriate intermediate standard within the limits set by the instrument manufacturer, refocus or recalibrate fol lowing the manufacturer's instructions. 10. Procedure 10.1 Bring the specimen to the instrument for measure ment. Be sure the specimen is flat. 10.2 For Test Method A, be certain that the specular sensor is centered on the spee'imeh-reflected specular light beam. One type of instrument, illustrated, in Fig. 1A, provides for screw-controlled movement, of the receptor assembly to achieve this centering. The full goniophotometer, shown in Fig. 2, identifies the specular direction by the peak of the goniophotometric curve. 10.3 Rotate the specimen in its own plane to fmd the orientation, giving the maximum specular signal. This spec imen orientation is called the "machine direction" because it 11. Calculation 11.1 For Test Method A, calculate the mean of three ti ll' readings for each specimen for. 11.1.1 Specular gloss, Rj30, at 30. 11.1.2 Distinctness-of-iniage gloss, 100 x (1 - 7/03), evaluated at 0.3" on either or both sides ofthe specular angle, 11.1.3 2 Reflection haze, 100 H2, evaluated at 2 on either or both sides of the specular angle. 11.1.4 5 Reflection haze, 100 Hs, evaluated at 5" on either or both sides of the specular angle. { 11.1.5 Directionality, 100 X (7^ acr0ss_macfl,inetl;;i Hi, with-machineX evaluated at 2" on either or both sides of the specular angle. 11.2 For Test Method B, calculate the mean of three readings of each specimen for: 11.2.1 Specular gloss, Rsi0 at 20". 11.2.2 One or more of the following, as required: 11.2.2.1 Reflection haze, H20. 11.2.2.2 Logarithmic reflection haze, H20loe = 1285 FIG. !2> Iog[(#2o/20) + 1]'. 11.2.2.3 Compensated reflection haze, H2o,COmp ~ ' G ' H2o , specimen - (Hn X Tsp-cimen/ Y,,). N' 3--H'm.io s may also be` calculated as a compensated quantity by using Ji2o, comp in Place of U20 in 11.2.212. Compensated quantities shall be used when comparing specimens with different values of Y. 12. Report f' a of cedt..r Bhffnthefy 12:1 The report for Test Method A shall contain the j||lMh lamriP following: 12.1.1 The specular gloss Rsj0, 12.1.2 The distinctness-of-image gloss, 12.1.3 The 2" haze, H2, ABLE IB; and of I' 12.1.4 The 5 reflection haze, Hs, 12.1.5 The directionality. 12.2 The report for Test Method B shall contain the following: 12.2.1 The specular gloss R2t2a, 12.2.2 Either the logarithmic reflection haze or the com pensated logarithmic reflection haze. 12.3 The report for both methods shall contain the following: 12.3.1 Identification of instrument used by model and gle of center llmeasured % . iperpendlcuE.. Jjsurface) |>; lipiwth (in the ^iangte of ingth (acroslr, fjthe angle of serial number. 1012 DUP050298190 of a sheet iss reflectance ness-of-image :ion haze, ffs. ' either glos^ heir ratios to i (a). ' 20 specula: the luminous amen, haze for the atten the test tse. a end of the trument has ML aan of three (1 - h 0a : iecular angle, ed at 2 on ed at 5 on across-machine/,,Jr i sides of the , :an of three *, AMPL/WZVC? COt/TAtOL UNIT &ZCOKDER WIT ired: *' m = 1285 J 20,comp sated quantity tied quantities atues of Y. contain the || FIG. 2 Recording Goniophotometer Showing Viewing Angle, v. Incidence Angle, i, and Their Respective Field Angles, 2KV and 2K, 1 |TABLE 1A Dimensions of the Mirror Image of the Source-Slit, and of the Receptor Windows Measured in the Plane of the Receiving Windows (see Fig. 1A) p I1- gjle of center of window (measured from, perpendicular pi specimen surface) Sjth (In the plane of the angle of reflection) jfgth (across the plana of the angle of reflection) Source-Slit Mirror Image, deg 30 0.44, 0.01 5,0 i Specular Receiver Window, deg 30 0.4 0.01 . 3.0 1 Distinctnass-of-lmage (*0.29) - -Receiver Window, deg 30.3 dnd '29.7 0.14 0.01 . r3.0 1 Haze Receiver - Windows, deg 28 and 32 or 25 and 35' 0.4 0.1 or 0.5. 0.1 3.0 1: ' s contain the ar the comlontain the model and | ' G ' IB Dimensions of the Specular Image of Ihe Source-Slit and of the Receptor Windows Measured in the Plane of the Receiving Windows (see Fig. IB) Source-Slit Specular Image, deg Specular Gloss Receiver Window, dag Haze Receiver Window, deg iple of center of window ^measured from perpendicular to specimen Surface) j|ph (in the plane of the |ingle of reflection) Igbgth (across the plane of |he angle of reflection) 20.0 0.1 0.75 0.1 2.5 0.25 20.0 0.1 1.8 0.05 3.6 0.1 18.1 0.1 and 21.9 0.1 1.8 0.1 5.5 0.25 12.3.2 Identification of gloss standards by number and scale value assigned, and 12.3.3 Identification of any specimens whose values on any scale differ by more than 3.0 in individual readings from the averages reported. 13. Precision and Bias 13.1 Test Method A: 13.1.1 An indication of the sensitivity of this test method is shown in Table 2 by the values of Spearman rank correlation coefficients. The data were obtained with a set of 20 aluminum and stainless steel specimens selected for a J013 DUP0502981 91 # E 430 FIG. 3 A Rotatable Clamp Suggested for Flattening the Specimen and Positioning It During Measurement TABLE 2 Rank Correlation Coefficients of Distinctness-of-lmage and Haze Between the Dori-Gon Abridged Goniophotometer and ,, Other Instruments, and with Visual Judgments Dori-Gon Versus Distinctnessof-lmage* Haze 2 deg 5 deg Visual D10-5 Gonio Alcoa DORI Alcoa Abridged Gonio D36B Dlstlnctness-of- (mage Gtossmetor 0.91 0.82 0.96 0.93 0.96 0.87 0.98 0.94 'Visual judgments of rank were,made by sighting in the "with" machine direction only, whereas Instrumental "with" and "across" directions were aver aged. a Visual judgments of haze were made by ranking the specimens according to the amount of near specular reflectance (milkiness} adjacent to We image of a concentrated light source. Correlation between the Dori-Gon and the D10-S Gonio and between the Doti-Gon and the Alcoa Abridged Gonio at 2 deg were equivalent to those at 5 deg. wide range of reflectance characteristics. Visual evaluations were compared with measurements using (1) the abridged goniophotometer, (2) a full goniophotometer, and (3) other instruments. A more complete report of these findings appears in Ref (5). TABLE 3 Instrument Reproducibility Data Root-Mean-Square Differences from Goniophotometer Assigned Values One instrument with receptor windows filled with optical fibers Average, two instruments with seg mented silicon photocell light receivers 30-deg Specular Reflectance 1.4 Distinctnessof-Reflecied Image 2.2 13.1.2 Instrument Reproducibility--Five panels of an odized aluminum sheet, ranging from 12 to 77 in speculrr reflectance and from 24 to 97 in distinctness-of-image gloss, ( were calibrated with the full goniophotometer, then mea sured with three abridged goniophotometers. One ol the abridged goniophotometers had optical fibers filling th. 1 receptor windows and two. instruments had receptor win dows of segmented silicon photocells. The results of the fa, goniophotometer calibration are given in Table 3. . 13.2 Test MethodB: 13.2.1 Precision and Bias will be determined. REFERENCES (1) Tingle, W. H., and Potter, F. R., "New Instrument Grades for Polished Metal Surfaces,'' Product Engineering, Vol 27, March 196!. (2) Tingle, W. H., and George, D. J., "Measuring Appearance Charac teristics of Anodized Aluminum Automotive Trim," Report No. 650513, Society of Automotive Engineers, May 1965. (3) Hunter, R. S., "Gloss Evaluation of Materials," ASTM Bulletin 1S6, ASTBA, December 1952. (4) Christie, J. S., "Instruments for Metallic Appearance," Appearance of. Metallic Materials, ASTM STP.478, Am. Soc. Testing Mats,, ASTTA, 1971. (5) Christie, J. S., "An Instrument for the Geometric Attributes < i 1 2 3 Metallic Appearance," Applied Optics, Vol. 8, No. 9, Septembi 1969. 1014 DUP050298192 DU PO 502 98193 Designation: G 6 - 88 Standard Test Method for Abrasion Resistance of Pipeline Coatings1 * This standard is issued under the fixed designation G 6; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (t) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 This method of accelerated test is a procedure for determining the relative resistance of steel pipeline coatings to abrasion by a slurry of coarse abrasive and water. The method is intended to apply to the testing of all types of electrical insulating pipeline coatings and tapes, including thermoplastics, thermoset, and bituminous materials. 1.2 Pipeline coatings are not normally subjected to the type of abrasion herein specified. 1.3 Metallic protective coatings such as zinc may be compared visually, but do not meet the electrical require ments of this test method. 1.4 This test method may involve hazardous operations and equipment. This test method does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this test method to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1.5 The values stated in SI units to three significant decimals are to be regarded as the standard. 2. Referenced Documents 2.1 ASTM Standards: G12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel3 G62 Test Methods for Holiday Detection in Pipeline Coatings3 3. Definition 3.1 holidays--small faults or pinholes which permit cur rent drainage through protective coatings on steel pipe. 4. Summary of Test Method 4.1 Apparatus and materials are described whereby coat ings on steel pipe are worn away by an abrasive slurry contained in a horizontally revolving drum. Specimens extend through both ends of the drum and are electrically insulated from contact with the test apparatus. 4.2 Periodic measurement of the electrical resistance be tween the specimen and the drum indicates the degree of 1 This test method is under the jurisdiction of ASTM Committee G-3 on Durability of Nonmctallic Materials and is the direct responsibility of Subcom mittee 003.06 on Durability of Pipeline Coatings and Linings. Current edition approved May 27, 1988. Published July 1988. Originally published as G 6 - 69 T. Last previous edition G 6 - 83. * Annual Book ofASTM Standards, Vols 06.01 and 14.02. 3 Annual Book ofASTM Standards, Vol 14.02. 3 Figure 80 [-V Jar Mill (U.S. Stoneware, Inc., Akron, OH) provides a suitable means for revolving the drum. abrasion resistance of the coating. 5. Significance and Use 5.1 This procedure defines a test method for comparing the relative resistance of pipeline coatings to abrasion. 5.2 Abrasion resistance may be used to specify optimum coating thickness of candidate materials both in develop ment and research work to study new coating systems or, methods and in quality control. 6. Apparatus 6.1 Drum--A cylindrical steel container suitable for testing nine specimens simultaneously. Figures 1 to 3 show construction details which may be altered at the cap as sembly if desired. A valve shall be provided to release any pressure built up during test, 6.2 Apparatus for Revolving the Drum--Any suitable apparatus used to revolve the drum at 30.48 m (100 linear ft)/min. A modifiedjar rolling mill3 has been found satisfac tory for revolving the drum. 6.3 Thickness Gage, to he used in accordance with Method G 12. 6.4 Holiday Detectors, low-voltage wet-sponge type for thin film coatings (coatings thinner than 20 mils), and high-voltage type for thick film coatings (coatings thicker than 20 mils). N' i--Low voltage detectors are used to locate pinholes, voids, or thin spots in pipeline coatings. The potential used with wet-sponge detectors can be up to 100 V DC. Procedures for using these detectors are found in Method A of G 62. For use of high voltage detectors. operating in the 900 to 20 000 Vdc range, see Method B of G 62, 6.5 Volt-ohm-meter--Any -electrical test instrument for measuring electrical resistance of the circuit. 7. Reagents and Materials 7.1 The test slurry shall consist of the following: 7.1.1 Aluminum Oxide Grit,4 13.6 kg (30 lb). 7.1.2 Tap Water, 5.68 L (116 gal). 8. Test Specimen 8.1 A 19.1 mm test specimen 406 mm (16 in.) long shall be prepared with its surface preparation and coating proce dures equivalent to that of production coated pipe. Only holiday-free specimens, in duplicate, shall be used in this test. n Exolon aluminum oxide abrasive, No. 3 mesh, Type TA, untumbled, available from Exolon Co., Tonawanda, NY 14150, has been found satisfactory for this purpose. 1016 8.2'D lecti<?4 1 Condi >9.1 T| 21tk JjeginiiirC.. (L Prof" 10.1 17 `C(7f *10.2 f; pecimef 10.3 fe etector|< > dam#: 10.5 |. brasivekf 10.6 | ealing t|>. pecimeJ neasuref ban inffe:. DUP050298194 l,0"niNG finHiC G6 iparmg L. timum svelopsms or;[ )le for 3 show ;ap asise any ratable 1 linear itisfac- . s with , Kpe for ,t ), and thicker Symbol A B G 0 E F G H 1 > K L M N Dimensions tor Fig. 1: mm 0.15 2.28 3.17 4.76 6.35 19.05 25.40 31.75 38.10 47.63 136.53 149.23 355.6 406.4 in. 0.006 0.090 0.125 0.188 0.250 0.750 1.000 1.125 1.500 1.875 5.376 5.875 14.0 16.0 N' --Estimated weight includes water and abrasive 39.5 kg (87 lb) FIG. 1 Abrasion-Tester Assembly 'oids, or -sponge electors electors 52. snt for. g shall proce- Only n this tumbled, dory for 8.2 Control specimens shall be included in each test, the ction of which is optional with the user. Conditioning 1-9.1 The specimen shall be exposed to a room temperature 21" to 25C (70 to 77"F) for a period of 24 h before |ginning the test.i. i. Procedure f 10.1 Perform the test' at a room temperature of 21 to C (70to 77F). i 10.2 Measure and record the coating thickness of each pecimcn in accordance with Method G 12. 10.3 Check all specimens or holidays using an appropriate etector. 10.4 Position the specimens in the drum taking care not ? damage the coating. 10.5 Load the apparatus with 13.6 kg (30 lb) of unused brasive and 5.68 L [ Vh gal) of water. 10.6 Test each specimen for electrical resistance after paling the drum by using the volt-ohm-meter. Immerse the pecimen in the slurry at the time the electrical resistance is neasured. Reject and replace any specimen showing less han infinite resistance. 10.7 Revolve the drum at the rate of 30.5 m (100 linear ft)/min. 10.8 Determine the electrical resistance at 25-h intervals for a test period of 200 h. 10.9 Relieve the pressure built up during the test by opening the release valve each time the electricalresistance is measured. -- 11. Report 11.1 The report shall include the following: 11.1.1 Complete identification of test specimens, in cluding name and code number of coating, size of the pipe, production date, production run number, and any other information that may be pertinent to identification, 11.1.2 Date of starting and of terminating the test, 11.1.3 Coating thickness of the test specimen before testing and minimum coating thickness after testing, 11.1.4 Volt-ohm-meter readings at 25-h intervals, and 11.1.5 Description of coating appearance after testing. 12. Precision 12.1 Precision data are limited to two adjacent specimens taken from the same production-coated pipe, assuming that the production process was uniform with respect to pipe 1017 f' DUP050298195 G6 ti, 1!s! if _ 11- id 1 ~i NoreWELO LEAK-PROOF Symbol A B B, c D E F' G H 1 J K L M N 0 P Q Dimensions for Rg. 2: mm 1.59 3.18 6.35 12.70 19.05 22.23 25.40 38.10 41.25 41.28 44.45 50.8 T27.0 165.1 266.7 304.8 349.25 . 355.6 FIG. 2 Drum in. 0.063 0.125 0.250 0.500 0.750 0.875 1.000 1.500 1.624 1.625 1.750 2.0 5.0 6.5 10.5 12.0 13.75 14.0 surface condition and coating material. Specimens that were not adjacent in the as-produced condition, or were taken from different lengths of pipe may represent differing process conditions. 12.2 Repeatability--When more than one test ofthe same coating material is involved, the standard deviation of the results should not be greater than 1.0 times the hourly time interval between inspections for the specific coating material. The standard deviation5 of a set of numbers is the square root of the average of the squares of the deviations of the numbers from their average. The standard deviation of two or more specimen results may be found by the following 5 For more information see the ASTM Manual on Presentation of Data and Control Chan Analysis. STP 15D, October 1976. procedure: Standard deviation, i \/n{(nSXZ-(ZX)2)'n\ where: XX = n-- <t = sum ofall values of X, from Xt to X,, inclusive, number of observed values (observations), and standard deviation, the root-mean-square (rms) deviation ofthe observed values from their average 12.3 Reproducibility--Agreement between laboratorie: should be such that the standard deviation of the results for a specific coating should not be greater than 1.5 times the inspection time interval. ?t jT. !f ( ll^ 1 < *" !- ii* 1018 DUP0502981 96 Symbol A a c D E 'F G H 1 j K L M N 0 P Q R . Dimensions for Fig. 3: mm 1.59 3.18 6.35 7.94 12.70 15.88 19.05 22.23 38.10 25.68 41.25 41J28 50.80 51.05 136.53 149.23 165.10 184.15 FIG. 3 Details in. 0.063 0.125 0.250 0.313 0.500 0.625 0.750 0.875 1.500 1.281 1.624 1.625 2.0 2.250 5.375 5.875 6.500 7.250 The American Society for Testing andMaterials takes ho position respecting the validity of ally patent rights assertedin connection with any item mentioned in this standard. Users of this standard-are expressly advised that determination ot the validity ot any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and ifnot revised, either reapprovedor withdrawn. Your comments are Invited either tor revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP050298197 Designation: 6 8 - 90 Standard Test Methods for Cathodic Disbonding of Pipeline Coatings1 This standard is issued under the fixed designation G 8; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. 1. Scope 1.1 These test methods cover accelerated procedures for simultaneously determining comparative characteristics of insulating coating systems applied to steel pipe exterior for the purpose of preventing or mitigating corrosion that may occur in underground service where the pipe will be in contact with inland soils and may or may not receive cathodic protection. They are intended for use with samples of coated pipe taken from commercial production and are applicable"to such samples when the coating is characterized by function as an electrical barrier. 1.2 This test method is intended for testing coatings submerged or immersed in the test solution at room temper ature. When it is impractical to submerge or immerse the test specimen, Test Method G 95 may be considered where the test cell is cemented to the surface of the coated pipe specimen. If higher temperatures are required, see Test Method G 42. If a specific test method is required with no options, see Test Method G 80. 1.3 The values stated in SI units to 3 significant decimals are to be regarded as the standard. . 1.4 This standard does not purport to address all of the safely problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to me. 2. Referenced Documents 2.1 ASTM Standards: G 12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel2 G 42 Method for Cathodic Disbonding of Pipeline Coat' ings Subjected to Elevated Temperatures2 G80 Test Method for Specific Cathodic Disbonding of Pipeline Coatings3 G95 Test Method for Cathodic Disbondment Test of Pipeline Coatings (Attached Cell Method)3 3. Summary of Test Methods 3.1 Both of the two test methods described subject the coating on the test specimen to electrical stress in a highly conductive, alkaline electrolyte. Electrical stress is obtained either by means of a sacrificial magnesium anode or from an 1 These test methods are under the jurisdiction of ASTM Committee G-3 on Durability of NanmetaUic Materials and arc the direct responsibility of Subcom mittee G03.06 on Durability of Pipeline Coatings and Linings. Current edition approved May 25, J 990. Published July 1990. Originally published as G 8 - 69 T. Last previous edition G 8 - 85. 2 Annual Book oj ASTM Standards, Vols 06.01 and 14.02. * Annual Book ofASTM Standards. VoJ 14,02. impressed current system. The coating is perforated before starting the test. 3.1.1 In Method A, a magnesium anode is used with no electrical monitoring during the test period. The results are determined by physical examination after the test period is concluded. 3.1.2 In Method B, either a magnesium anode or an impressed current system may be used. Electrical instrumen tation is provided for measuring the current in the cell circuit. The electrical potential is also measured, and upon conclusion of the test period, the test specimen is physically examined. 3.1.3 In both test methods physical examination is con ducted by comparing the extent of loosened or disbonded coating at the perforations in the immersed area with extent of loosened or disbonded coating at a new test hole in the coating made in an area that was not immersed. 4. Significance and Use 4.1 Breaks or holidays in pipe coatings may expose the pipe to possible corrosion, since after a pipe has been installed underground, the surrounding earth will be more or less moisture-bearing and it constitutes an effective electro lyte. Damage to pipe coating is almost unavoidable during transportation and construction. Normal soil potentials as well as applied cathodic protection potentials may cause loosening of the coating, beginning at holiday edges, in some cases increasing the apparent size of the holiday. Holidays may also be caused by such potentials. While apparently loosened coating and cathodic holidays may not result in corrosion, this test provides accelerated conditions for loos ening to occur and therefore gives a measure of resistance of coatings to this type of action:-- 4.2 The effects of the test may be evaluated by either physical examination or monitoring the current drawn by the test specimen or both of, these two. Usually there is no correlation between the two methods of evaluation but both methods are significant. Traditional physical examination consists of assessing the effective contact of the coating with the metal surface in terms of observed differences in the Relative adhesive bond. It is usually found that, the electrically stressed area propagates from the holiday to a boundary where the loosened coating leaves off for the more effective contact or bond attributed to an original condition throughout the specimen before electrical stressing was applied. Assumptions associated with test results include the following: 4.2.1 Attempting to loosen or disbond the coating at a new test hole made in the coating in an area that was not immersed represents maximum adhesion or bond as mea sured by the lifting technique used, and that the same lifting u :l(ipinique \ "Cieieby Ip: i rto lifting. , >', 4.2:2 A , ftiist holes ' not ,, ] RocessjA;'. I'tcoinparp' .pt necessT' that allk Ssbontj I?faring ot? ' portan;:-, Ithers anc:: lating s^j; Ion protif; " 4.2.3 1;; hdicator|:.; ipuosioifl' iS much|i ferotectiof" 1020 DUP050298198 if t. ` ,4#i aefo $ 'a * no j tsare iod is'sj >r an meni i] upon icnlh ' rou nded dent i the SPECIMEN SUPPORTED 8Y the ieen, eor troing i as use me ays itly in os<>r ier l;y no th 5n tli le ly <7 'e n is e | N' --Test \ j made in non-immersed area after testing not shown (see Fig. 5). PIG. 1 Test Assembly for Method A Using a Magnesium Anode nique can be used at a test hole that was immersed iby providing a means of'Comparing relativb resistance |> lifting. ' 4.2.2 Any relatively lesser bonded area at the; immersed ist holes in the coating was caused by electrical stressing and /as not attributable to an anomaly in the application irocess. Ability to resist disbondment is a desired quality on comparative basis, but disbondment tier se jn this test is ot necessarily an adverse indication. The virtue of this test ; that all dielectric type coatings now in corhmon use will isbond to some degree thus providing a means of com- Jparing one coating with another. Bond strength is more Important for proper functioning of some coatings than others and the same measured disbondment fortwo different [coating systems may not represent equivalent loss of corro sion protection. | 4.2.3 The amount of current in the test cell js a relative y indicator of the extent of areas requiring protection against ^ corrosion; however, the current density appearing in this test " is much greater than that usually required for cathodic protection in natural, inland soil environments. 5. Apparatus 5.1 Apparatus for Both Methods: _ 5.3.1 Test Vessel--A nonconducting material .shall be W used for the vessel or as a lining in a metallic vessel. Dimensions ofthe vessel shall permit the following require ments: 5.1.1.1 Test specimens shall be suspended vertically in the vessel with at least 25.:4-mm (1-in:) clearance from the bottom. 5.1.1.2 Each test specimen shall be separated from the other specimens,' from the anodes and from the walls of the test vessel by at least 38.1 mm (1.500 in.). 5.1.1.3 Depth of electrolyte shall permit the test length of the specimen to be immersed as required in 7.4. 5.1.1.4 If electrical monitoring is to be performed as required in Method B, the reference electrode may be placed anywhere in the vessel, provided it is separated from the specimen and from the anode by not less than 38.1 mm (1.500 in.). 5.1.2 Magnesium Anode--The anode shall be made of a magnesium alloy having a solution potential of -- 1.45 to -1.55 V with respect to a CuCuS04 reference electrode in the electrolyte given in 6.1. It shall have a surface area not less than one third that of the total specimen area exposed to electrolyte (outside area exposed only). The anode shall be provided with a factory-sealed, 4107-cmil (14-gage Awg), minimum, insulated copper wire. Anodes without a factory seal may be used if the magnesium extends above the cover. 5.1.3 Connectors--Wiring from anode to test specimen shall, be 4107-cmil (14-gage Awg), minimum, insulated copper. Attachment to the test specimen shall be by sol- 1021 I DUP050298199 G8 -' < { ' '< (' VOLTMETER V- HIGH-RESISTANCE + - VOLTMETER OR POTENTIOMETER ONE OHM/ RESISTOR / ALLIGATOR CLIP OR KNIFE SW. TERMINAL BOARD ri ro PrT - NON CONDUCTIVE COVER -IMMERSION LINE REFERENCE ELECTRODE INTENTIONAL HOLIDAY ELECTROLYTE ------------- TEST VESSEL SPECIMEN -MAGNESIUM ANODE FIG. 2 Test Assembly for Method B Using a Magnesium Anode dering, brazing, or bolting to the nonimmersed end, and the place of attachment shall be coated with an insulating material. A junction in the connecting wire is permitted, provided that it is made by means of a bolted pair of terminal lugs soldered or mechanically crimped to clean wire ends. 5.1.4 Holiday Tools--Holidays shall be made with con ventional drills of the required diameter. For use in pJc. paring small-diameter pipe specimens such as 19.05 mm (0.750 in.) nominal diameter pipe, the use of a drill modified by substantially grinding away the sharp cone point has been found effective in preventing perforation ofthe metal wall of the pipe. A sharp-pointed knife with a safe handle is required for use in making physical examinations. 5.1.5High-Resistance Voltmeter, for direct current, ' having an internal resistance of not less than 10 MO and having a range from 0.01 to 5 V for measuring potential to the reference electrode. 5.1.6. Reference Electrode, saturated CuCuSO., of conven tional glass or plastic tube with porous- plug construction, i preferably not over 19.05 mm (0.750 in.) in diameter, having a potential of -0,316 V with respect to the standard F hydrogen electrode. A calomel electrode may be used, but |f; measurements made with it shall be converted to the : CuCuS04 reference for reporting by adding -0.072 V to the observed reading. 5.1.7 Thickness-Gage, for measuring coating thickness in accordance with Test Method G 12. 5.1.8 Thermometer, for measuring electrolyte tempera- - ture, general lab type, T subdivisions, 76.2 mm (3 in.) immersion. 5.2 Additional Apparatusfor Method B: 5.2.1 High-Resistance Voltmeter, for direct current, j having an internal resistance of not less than 10 Mil and 5 capable of measuring as low as 10 gV potential drop across a j shunt in the test cell circuit. } 5.2.2 Precision Wire-Wound Resistor, 1-Si 1 %, l-W (minimum), to be used in the test cell circuit as a shunt for; current. . 5.2.3 Volt-Ohm-Meter;, for initial testing of apparent coating resistance. 5.2.4 Metallic Electrode, used temporarily with the volt- ohm-meter to determine apparent initial holiday status of* the test specimen. 5.2.5 Additional Connecting Wires, 4107-cmil (14-gage - HIGH- - +" 4- RESISTANCE VOLTMETER t -- HIGH-RESISTANCE ----- VOLTMETER OH + -I POTENTIOMETER TERMINAL BOARD more tft5 NONCONDUCTIVE COVER IMMERSION LINE REFERENCE ELECTRODE INTENTIONAL HOLIDAY ELECTROLTTE TEST VESSEL IMPRESSED CURRENT ANODE FIG. 3 Test Assembly tor Method B Using an Impressed Current with One Specimen 1022 m DUP050298200 r- For use in Pre. uch as 19.05 ttlg| of a drill modify! one point has beJj )f the metal wall of handle is requir^ direct current I than 10 Mfi antfif "ring potential to| CuS04 of conven- L riug construction 1 i diameter, having " to the standard jl may be used, but f inverted to the ' ; -0.072 V to the Set rectifier output volloge to not over 3 volts; Ihtn trim each voltage divider so thot & lo C measures1.5 volts. 7I OHM RESISTORS I % ACCURACY SPECIMENS --. s'RECTIFIER /-----lOO OHM, 25 WATT RHEOSTATS a.{`VOLTAGE DIVIDERS) > 9G ( \.. [___> ating thickness id jj arolyte tempera'6.2 mm (3 in.) cz>-nl..~... --V direct current, han 10 MSI and rial drop across a To meosure current use terminals A and 8 To measure voltage use terminals A ondC '-REFERENCE ELECTRODE FIG. 4 Modification of Method B (Fig. 3) Using Impressed Current to Test More than One Specimen -0 1 %, ],\y . it as a shunt for ig of apparent y with the voltoiiday status of 7-cmiI (14-gage |/g), minimum, insulated copper. 6.2.6 Brass Studs, used at a terminal board, together with ligator clips or knife switches, for making and breaking |cuits. Alligator clips shall not be used to connect to ctrodes or specimens at the top location of test cells. |5.2.7 Zero-Resistance Ammeter, capable of measuring greet current as low as 10 itA may be used in the alternative gjethod given in 9.1.3 and substituted for the apparatus scribed in 5.2.1 and 5.2.2. f 5.2.8 Direct-Current Rectifier, capable of supplying conant voltage at a voltage of 1.50 0.01 V, as measured ptween the specimen and reference electrode. 15.2.9 Impressed Current Anode, shall be of the jjbnconsumable type provided with a factory sealed,, insu lted copper wire.4 5.2.10 Voltage Divider, 100-9, 25-W rheostat, to be used (more than one specimen is to be tested as shown in Fig. 4. Reagent and Materials 6.1 The electrolyte shall consist of potable tap water with he addition of l mass % of each of the following technical|rade salts, calculated on an anhydrous basis: sodium chlode, sodium sulfate, and sodium carbonate. Use freshly prepared solution for each test. 6.2 Materials for sealing the ends of coated pipe specijjtnens may consist of bituminous products, wax, epoxy, or either materials, including molded elastomeric or plastic end [caps. 6.3 Plywood or plastic material has been found suitable for the construction of test vessel covers and for the support through apertures of test specimens and electrodes. Wood dowels introduced through holes in the top ends of test specimens have been found suitable for-suspending test specimens from the vessel cover. : 7. Test Specimen , 7.1 The test specimen shall be a representative piece df production-coated pipe. One end shall be plugged or capped, and sealed. 7.2 One or three holidays shall be made-in each specimen. Three holidays are recommended. Recommended dimen sions are given in Fig. 5. A specimen with one holiday shall have it drilled in the middle of the immersed length. If three holidays are used, they shall be drilled 120 apart with one in the center and the other two at locations one fourth the distance from top and bottom of the immersed test length. Each holiday shall be drilled so that the angular cone point of the drill will fully enter the steel where the cylindrical portion of the drill meets the steel surface. The drill diameter shall be not less than three times the coating thickness, but it shall never be smaller than 6.35 mm (0.250 in.) in diameter. The steel wall of the pipe shall not be perforated. With small- i diameter pipes, where there is danger of perforating the pipe, the holiday shall be started with a standard 60 cone point and finished with a drill that has had a substantial portion of the cone point ground away. 4 Durioii. a material found suitable for this purpose is available from Durion |Co., Inc., Dayton OH. N' 1--Before making the holiday, see 8.1. ' 7.3 The end of the pipe which will protrude above the 1023 DUP0502 98201 ^peolnj pipe: "pjcatoi. <v Star fl 114.3 6.35 233.363, min 19.05, min 762, min ;( 4.500 0.250) { 9.1875, min) ( 0.750, rhin) (30, min); FIG. 5 Recommended Dimensions for Specimen immersion line shall be, provided with suitable supporting mean? and a separate wire connection for electrical purposes, soldered, brazed, or bolted to the pipe. The protruding end, including hanger and wire connections, shall be protected and sealed with an insulating coating material. 7.4 The specimen test area shall consist of the area between the edge, of the bottom end seal and the immersion line. The bottom end seal area shall not be considered part of the area tested. Any suitable diameter arid specimen length of pipe may be used, but the immersed area shall be not less than 23 227 mm2 (36 in.2). An area of 92 900 mm2 (1 ft2)' has been found preferable when convenient.8 8.Specimen Preparation 8.1 Before making artificial holidays, verify the continuity of the coating and the effectiveness of the end-cap seal as follows: 8.1.1 Immerse the test specimen and a metallic electrode in the electrolyte. Connect one terminal of the multimeter to the test specimen and the other terminal to the metallic electrode. Measure the apparent resistance in ohms, making two determinations: one witjithe specimen connected to tbi positive terminal of the multimeter; and one with thi specimen connected to the negative terminal. 8.1.2 Disconnect the specimen from the multimeter but leave it immersed for 15 miti. Then-measure the resistana again as in 8.1.1. 8.1.3 A significant decrease in either resistance reading after 15'min will indicate a flaw in the coating or end-cap -seal! Reject the specimen if the `flaw is identified in the coating. If the flaw is in the end-cap seal, it may be repaired and the resistance remeasured as in 8.1.1 and 8.1.2. 8.1.4 The lowest resistance after 15 min of immersion shall be not less than 1000 M2 but a stable reading below 1000 Mil may not indicate a flaw and the specimen may be usbd for''test. All resistance measurements shall be reported in the results. 8.2 Record initial holiday diameter(s). 8.3 Measure and record the minimum and maximum coating thickness in accordance with Method G 12, and the 1024 'Reijtifi i; IjeotiSejjl ( fthick n^S'.., 4;' . Prof 9-1 11 |connect middle: Space l>{ in sag = |speciiT|;. Itions f. lelectroR? 9.1. p jmeasufr lelectrt: {before^; Imentafe'. MiNi DUP050298202 9 G8 Data Sheet and Report, Part I, for Method A and Method B Cathodic Disbonding of Pipeline Coatings ------------------- Report No. Initials .. Date. . mm (in.) O.D._ mm (in.) Wall- mm (in.) Length ihod :IW Av. At holidays: Top . Middle Bottom Date finished . mm2 (in.2) Initial holiday dia. mm (in.) Final unsealed area mm2 (in.2) (--) Initial holiday area mm2 (in.2) * Net disbonded area mm2 (in.2) Disbonded Equivalent Circle Diameter mm2 (in.2) Top Middle 5. Preliminary verification Bottom Average Largest Disbonded Equivalent Circle Diameter (ECD) does not exceed Spontaneous Holidays * -12.7 v 25.4 38.1 50.8 More than 50.8' 0:50 1.00 ; 1)50. 2.00 More than 2.00 None None None None Any Verification of coating continuity before starting test per Sec. 7.6 Megohms Trial Polarity Initial After 15 min. Initial Final Plus Minus Plus Minus urrent: nt<was qot continuous indicate interrupted time (min., hrs.): FIG. 6 Suggested Form, Part I, for Use in Presenting Data tor One Specimen Method.A and Beihod B Inhere each holiday is made. ure for Method A erse the test specimen in the electrolyte and to the anode as shown in Fig. 1. Position the single holiday soithatit faces away from the anode, 'anode with respect to test specimens as described Mark the correct immersion level of the test ' with a grease pencil and maintain by daily addipotable water as required. Perform the test at temperature of 21 to 25C (70 to 77F). order to ascertain that the test cell is functioning, l"e potential between test specimen and a reference (mediately after starting the test and immediately ainating it. Use temporary connections and instruas shown in Fig. 1. The potential measured shall be -1.45 V to -1.55 V with respect to a CuCuS04 reference electrode. Use the instrument described in 5.1.5. 9.2 Duration of the test period shall be 30 days. Option ally, other test periods such as 60 or 90 days may be used. 9.3 An examination shall be performed immediately upon termination of the test period as follows: 9.3.1 At the end of the test period, disassemble the cell and rinse the test area with warm tap water. Immediately wipe the sample dry and visually examine the entire test area for any evidence of unintentional holidays and loosening of coating at the edge of all holidays, including the intentional holiday, and record coating condition, for example, color, blisters, cracking, crazing, adhering deposits, etc. 9.3.2 Drill a new reference holiday in the coating in an area that was not immersed. Follow the same drilling procedure as described in 7.2. 1025 DUPO 502 98203 G8 Data Sheet and Deport, Part It, for Method S Cathodic Disbonding of Pipeline Coatings Electrical Monitoring, Method B initial Ohms + _ Elapsed days of 1 DateandTlme Test, 70 j Potential to Ref., V Actual jxA mVf2 e, = 4 Average Values on Target Dates A, V MA H log (, - -* Charge, Start to Termination: Far the specimen: per Initial Holiday: Av FIG. 7 Suggested Form, Part II, for Use In Presenting Data for One Specimen, Method B 9.3.3 Make radial 45 cuts through the coating inter secting at the center of both the intentional holiday and the reference holiday with a sharp, thin-bladed knife. Take care to ensure that coating is cut completely through to the steel substrate. 9.3.4 Attempt to lift the coating at both the reference holiday and the intentional holiday with the point of a sharp, thin-bladed knife. Use the bond at the reference holiday as a reference For judging the quality of the bond at the inten tional holiday. Measure and record the total area of disbonded coating at the intentional holiday. N' 2--The use of a transparent film having a grid laid out in small squares such as 2.54 mm (0.1 in.) on a side has been found useful. The film is placed against the unsealed area and the boundary of the unsealed area traced on the grid. The area is then obtained by counting the squares within the bonded area.10 10. Procedure for Method B 10.1 In addition to the procedure given in Section 9, monitor the progress of the test electrically in accordance with the schedule given in 10.2 as follows: 10.1.1 If a magnesium anode is to be used, install the test assembly shown in Fig. 2. If impressed current for a single specimen is to be used, install the test assembly shown in Fig. 3; if more than one specimen is to be tested, use the modification shown in Fig. 4. 10.1.2 Measure E2, the stress potential in volts between test specimen and reference electrode, with a multimeter without disconnecting the anode from the test specimen. Use the instrument described in 5.1.5. If a CuCuS04 electrode is used, immerse only temporarily. 10.1.3 Measure /,, the current demand in amperes, by determining the potential drop across the 1-S2 resistor perma nently installed in the test cell circuit with the multimeter described in 5.2.1. The voltage reading will be numerically equal to amperes. N' 3--An alternative method of measuring current demand may be used by means of the instrument described in 5.2.4. In this method, the jyire connection between test specimen and anode is temporarily broken and a zero-resistance ammeter temporarily interposed between the specimen and the anode. Reconnect the specimen to the anode with the connector wire as soon as this measurement is completed. this with the multimeter described in 5.1.5 connected between the test specimen and the reference' electrode'as follows: .....-- 10.1.4.1 Disconnect the anode from the test specimen while closely observing the multimeter. As the instrument pointer falls, it will dwell significantly at the polarized value before receding further. The dwell point is . If a CuCuS04 electrode is used, immerse only temporarily. : 10.2 Electrical Monitoring Schedule: 10.2.1 Eleotrical measurements at the start of the test are defined as the average of measurements taken on the second and third days after immersion. Measurements may be taken on the day of immersion in order to ascertain functioning of the test ceil, but such measurements are not to be used in calculating the change in characteristics from start to target dates in the conduct of the test. 10.2.2 Make electrical measurements at the start of a test and on a target date after 30 days. The test may be continued for 60 or 90-day targets with intermediate and corresponding electrical measurements. 10.2.3 Take electrical measurements for intermediate 1026 isctijic nents: 11.2.: DUP050298204 G8 get dates and for the terminal date on 2 successive days |r to and including the target date. The average of lings taken on the 2 days is defined as the target date fsurement. 6.2.4 Rectifier current shall be continuous. Any interlions must be reported. Report (see Figs. 6 and 7): i. 1 The report for Method A shall include the following: 1.1.1 Complete identification of the test specimen, in ping: l. 1.1.1 Name and code number of the coating, 1.1.1.2 Size and wall thickness of pipe, 1.1.1.3 Source, production date, and production run iber, il. 1.1.4 Minimum-maximum coating thickness, average ikness and the thickness at the holiday, 1.1.1.5 Immersed area, 1.1.1.6 Size and number of initial holidays, and 1.1.1 .;7 Resistance measurements verifying continuity of coating and effectiveness of the end cap seal as required 8.1. 11.1.2 Dates of starting and terminating test. 1.1.3 Tally of areas that have been found unsealed on the fminal date. Areas may be reported in square millimetres mare inches) or millimetres (inches) of equivalent circle meter of the area, or both. If more than one holiday was jtied, the area per holiday may be reported as an average. f'NoTE 4--Equivalent Circle Diameter (ECD) is obtained from the ma- j Simula: teter :ally, *1 jtiere: ECD = {Aj0.785)'* = area of holiday, mm2 (in.2) may 11.1.4 ther information that may be pertinent. ihod. (* 11.2 The report for Method B shall include the following: Ttrily I 1.2.1 The data required in the report foe Method A, Iween 11.2.2 The relative resistances of the test specimen in with lims before the artificial holiday was made as described in jj.1.4, and | 11.2.3 The results of starting, intermediate, and terminal electrical measurements. Report the following measure- fnents: : 11.2.3". 1 Current demand in microamperes, or negative nen lent due S04 characteristic of the logarithm of the current in amperes, or both, 11.2.3.2 The value of AE -- E2 -- in volts, and 11.2.3.3 Change from start to termination for values 11.2.3.1 and 11.2.3.2. If more than one holiday was used the average change per holiday may be reported for 11.2.3.1. 11.2.4 Any interrupted time of the rectifier current. 12. Precision and Bias 12.1 Precision data are limited to two adjacent specimens taken from the same production-coated pipe and assume that the production process was uniform with respect to pipe surface condition and coating material. Specimens that were not adjacent in the as-produced condition. or were taken from different lengths ofpipe may represent differing process conditions. The following data should be used forjudging the acceptability of results: (These precision data are approxima tions based on limited data, but they provide a reasonable basis forjudging the significance of results.) 12.2 Method A: 12.2.1 Repeatability--Duplicate results by the same worker should not be considered suspect unless they differ by more than 12.7 mm (0.5 in.) in value ECD in accordance with the following equation: ECD = U/0.785)'A where: A = unsealed area developed from 1 artificial holiday, mm2 (in.2). 12.2.2 Reproducibility--The results reported by one labo ratory should not be considered suspect unless they differ from those ofanother laboratory by more than 25 mm (1 in.) for value ECD in the equation given in 12.2.1. 12.3 Method B: 12.3.1 Repeatability--Duplicate results by the same worker should not be considered suspect unless they differ by more than unity in the negative characteristic of the loga rithm of the current demand in amperes. 12.3.2 Reproducibility--The results reported by one labo ratory should not be considered suspect unless they differ from those of another laboratory by more than unity in the negative characteristic of the logarithm of the current de mand in amperes. '-- test ued ling 1027 f DUP050298205 # G8 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in-this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either forrevision of this standard or for additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. Serf. \ 1-1 ] ate ' ^applied a? L21' egardl Jr L3 mttiohsn wddfesi m4 i wprdpi 'rnplm- 2.1*' <3-12 Fit, .fa. Siiif i 3.1 ilppe Si - nhe du ' jjoatini. Rhe wa ] `4. Sig Si j intinta |tionite; DOistUi. its M ihe tef|u ' eharac 'f? jjto it*efefwatdrf- |in Ifmateriif; ; If [5. Ap|| .hContai|! permiftS 5.1js ' least 1028 DUP050298206 Designation: G 9 - 87 Standard Test Method for Water Penetration into Pipeline Coatings1 This standard is'issued under the fixed designation G 9; the number immediately following the designation indicates the year of originaj adoption or, in.the case of revision, the yeanoflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {<) indicates an editorial change since the last revision or reapproval. Scope 1.1 This method covers the determination ofthe apparent ate of depth of water penetration into insulating coatings jjpplied to pipe. 1- T.2 The values' stated ih inch-pound units are to be geegarded as the? standard. 1.3 This standard may involve hazardous materials, oper ations,' and equipment: This standard''does not purport to address all ofthe safety problems associated with its use. It is Jkfie responsibility of the user of this standard to establish mappropriate safety and health practices and determine the |japplicability ofregulatory limitations prior to use. |.2, Referenced Document 2.1 ASTM Standard: G12 :Test Method for Nondestructive Measurement of ,, Film Thickness of Pipeline Coatings on Steel2 jt>3. Summary of Method '3.1 The method consists of an immersion-type test where pipe specimens are suspended in ah aqueous electrolyte for Ithe duration of the test period. Electrical measurements of Icoating capacitance and dissipation factor are used to follow ithe water absorption rate Of the test materials. 1`4. Significance and Use 4.1 The deterioration of an insulating coating film is . intimately related to its moisture content. The water penetraf-tion test provides a means for monitoring the passage of jmoisture through a coating material by means of changes in Bits dielectric constant. When expressed in relation to time, the test data will reflect a rate of deterioration which is a 3a characteristic of the coating material and will bear a'relatioii to its expected useful life as an insulating coating. The test for |water penetration will also provide information that is useful |in establishing the optimum coating thickness for a given s material. j 5. Apparatus i 5.1 Immersion Cell--Any suitable rionmelallic vessel to j contain the test specimens. Dimensions of the vessel shall , permit the following requirements: 5.1.1 Test specimens shall be suspended vertically with at least 25 mm (1.0 in.) clearance from the sides and bottom. 1 This method is under thejurisdiction of ASTM Committee G-3 on Durability of Nonmetallic Materials and is the direct responsibility of Subcommittee G03.06 on Durability of Pipeline Coatings and Linings. Current edition approved May 29, 1987. Published July 1987. Originally published as G 9 - 69 T. Last previous edition G 9 ~ 82. 2 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 5.1.2 Test specimens shall be separated by not less than 25 to 40 mm (1 to 1.5 in.) and a vertically suspended anode shall be placed at an equal distance from each specimen not less than the separation of distance. 5.1.3 The test vessel shall be deep enough to allow for immersion of the samples in the electrolyte to the level specified in 8.1. N' 1--Commercially available, glass battery jars in 2-dm3 (0.55- gal) and 10-dm3 (2.7-gal) sizes can be conveniently used with 19-mm (0.75-in.) and 5i-mm (2.0-in. nominal) diameter specimens, respec tively. 5.1.4 A suitable sample support plate fabricated from a material having a low dielectric constant shall be used to suspend the samples and anode above the immersion cell. The support plate shall contain an access hole for the reference electrode. A typical test cell is illustrated in Fig. I. 5.2 Electrolyte, consisting of tap water with the addition of 1 weight % of each of the following technical-grade anhydrous salts: sodium chloride, sodium sulfate, and so dium carbonate. N' 2--Add 30 g (1.05 oz) of sodium chloride for each dm3 (0.26 gal) of water. 5.2.1 The electrolyte in the immersion cell shall be maintained at the proper level by regular additions of tap water. The electrolyte shall not be reused after completion of the test. 5.3 Voltage Source--A direct current power supply, ca pable of supplying low ripple voltage shall be used to maintain a potential difference of 6.0 0.1 V dc between each of the test specimens and a common electrode. 5.4 Connectors--Wiring connections from the anode to the specimen shall be of No. 18 AWG insulated copper. Attachment to the anodeshall be sealed and kept above the level of the electrolyte. Attachment to the specimen shall be made by a method that will allow disconnection from the aflode when the measuring bridge is in use. A convenient means for accomplishing this is through the use of insulated pin-type jacks. 5.5 Capacitance Bridge3--Measurements of equivalent specimen capacitance and coating dissipation factor shall be made with a low-voltage a-c, resistive-ratio-arm type mea suring bridge having the following characteristics: 5.5.1 Oscillator frequency, 1 kHz 2%, 5.5.2 Series capacitance range, 1 to 1100 pF 1 %, 5.5.3 Series capacitance sensitivity, 0.5 pF, 5.5.4 Dissipation factor range, 0.001 to 1.0 at 1 kHz, and 5.5.5 Dissipation factor sensitivity, 0.001 at 1 kHz. 3 A bridge found to meet the requirements specified is the General Model 1656 Impedance Bridge, QenRad, Concotd, MA 01742. 1029 DUP050298207 # Q9 CLAMP. SAMPLE SUPPORT I -"PLATE AND CELL \t< COVER. FILLING HOLE COMMON ELECTROOE SUPPORT PIN ELECTROLYTE comparison circuit of the measuring bridge. Connection of the unknown to the measuring bridge shall be made in such a manner as to eliminate the introduction of stray capaci tance into the measuring circuit. A diagram for connectin. the test cell to the bridge is shown in Fig. 2. In tins arrangement, both the test leads are shielded and the chas,is of the bridge is grounded. The immersion cell shall also 1 e shielded to avoid capacitance effects from surroundini> objects. ' N' 3--A. shield for the test cell can conveniently be fabricated > from most commercially-available tin or aluminum foils of approxi inately 0.0382-mm (0.0015-in.) thickness and 'fbrmed arottnd di container. .. 5.7 Thickness Gage--Measurements of coating thickness will be required for this test. Any instrument suitable for use with Test Method G 1,2 can be.used.' 5.8 Anode, fabricated from 4.76-mm (0.1875-in.) diam eter AISI Type 303 stainless-steel rod, and shall be 178 mm (7.00 in.) long, with the upper 50 mm (2.00 in.) threaded to accept a locking nut. * ,i, . . BATTERY JAR LOWER END CAP FIG. 1 Typical Test Cell 5.6 Measuring Circuit--Measurements of specimen ca pacitance and coating dissipation factor shall be made using a circuit that places the sample unknown in series with the 6. Test Specimen 6.1 The test specimen shall be a representative piece ol production-coated pipe and shall be free of obvious coaling flaws or defects (see Fig. 3). Any suitable diameter anc specimen length can be used. Physical Emitations of the immersion cells suggested in 5.1.3, Note !, make it necessarj to restrict the over-all sample length to approximately 300 mm (12.0 in.) for both the 26.7-mm (0.75-in. nominal) and 60.3-mm (2.0-in. nominal) diameter coated pipe specimens; 6.2 The upper and lower ends ofthe test specimen shall be plugged and sealed with tiopconductive caps of sufficieni bulk to minimize effectively capacitive end effects in the measuring circuit. For this purpose, an end-cap thickness of TEST LEAD SHIELDS R< t ' --b| ti uni 13.1 lintainl. It2-1 1' |the rat exhij ily av| I well St150j t|; ilds ail'; rable|s| SAMPLE # I COTE uireditg b sn-wa COATING G-ow ) BRIDGE CHASSIS rXrr FOIL "-"-I SHIELD 11 IMPEDANCE BRIDGE S'GROUND ELECTRODE ELECTROLYTE FIG. 2 Connecting the Test Cell to the Bridge 1030 | PrelimeK |7.1 Cc|:. Sickness 17.2 Spifc, |posed cf P7.3 lith the DUP050298208 G9 Xtior of * in such ' capacianecting In this 3 chassis also tv ounding ' .'abrical^J , ' approxi)und the lickness ^ for use ) diam- < aded toi"" STO. MACHINE SCREW COATING ABOVE MOISTURE SHIELD TO BE COVERED WITH ENO-CAP MATERIAL. ) MINIMUM THICKNESS, T, FOR ENO-CAP TO BE 15 (V2) >iece of coating er and of the cessary sly 300 ' al) and . !imenssj,.,j shall be i fficient in the ness of prE--Dimensions are In millimetres with inches in parentheses. FIG. 31 Detail Drawing of Pipe Specimen 13 mm (0.5 in.) to 19 mm (0.75 in.) shall be Sntained. , j.2.1 The end-cap material shall have a dielectric constant he range from 2 to 6, bond well to the coating surface, exhibit a low water-absorption rate. Several commer- |ly available poly(vinyl chloride)-paraffin compounds,4 Jwell suited for this purpose. They have a melting point in : 150 to 200C (300 to 390F) range, can be poured into lids around the pipe sample, and appear as resilient, able solids at room temperature. N' 4--Using these materials, the end-caps can be applied to the iired thickness by repeated dipping of the sample ends into a Bten-wax bath, or through the use of light-weight, disposable molds of gjninum foil or paper formed around the pipe sample to allow the ling of the caps directly to the surface of the coated pipe sample. 16.3 The end of the specimen which will protrude above i immersion line shall be provided with a suitable means gjsupport and a separate wire connection for electrical poses. The protruding end of the sample shall be waterlofed with a thin coating of end-cap material (see Fig. 1). Energize the impedance bridge and measure the series capacitance, Cc of the lower end cap. 7.4 Initial Coating Capacitance--Add additional electro lyte to the immersion cell until its level reaches the lower edge of the upper end cap. Immediately measure and record the initial series capacitance, C0, and dissipation factor, DF, of the specimen, 8. Procedure 8.1 Energize each specimen by connecting it to the negative side of the voltage source. Keep each sample energized and immersed to the lower edge of the upper end cap for the duration of the test period. Maintain the specified electrolyte level through regular additions of tap water. 8.2 Throughout the test make periodic measurements of the series capacitance and dissipation factor ofthe immersed specimens in the following mariner: 8.2.1 Temporarily disconnect the test specimen from the voltage source. Verify that the electrolyte is at the proper level within the immersion cell. Connect the measuring bridge between the test specimen and stainless-steel anode. Energize the bridge and measure the series capacitance, C, and dissipation faction, DF, of the test specimen. 8.2.2 Using the observed value of series capacitance, Cs, calculate the- apparent depth of water penetration by the method described in 9.2. 8.2.3 Repeat the measurements of series capacitance and specimen dissipation factor at periodic intervals throughout the duration of the test. The frequency of measurement will depend upon the rate of deterioration of the coating sample. Where the water penetration process is relatively rapid, daily readings of sample capacitance and dissipation factor will be required. Normally, readings made at weekly intervals will adequately define the penetration rate. N' 5--Some coatings exhibit an initial rise in capacitance and dissipation factor, but reach a state of equilibrium in 6 to 9 months. An increase in capacitance and dissipation factor following this period of equilibrium, (or failure to reach equilibrium) indicates impending failure. A sample can be considered to have failed when the dissipation factor reaches a value of 1.0. 9. Calculations 9.1 Dielectric Constant--Calculate the dielectric constant, K0, for the coating film as follows: (C0 - Cr) In I(2tf! + d)/d] 0 NL (Preliminary Test Measurements . 1 Coating Thickness--Measure and record the coating . lekness by referring to Method G 12. 1.2 Specimen Length--Measure and record the length of iposed coating surface, between the end caps. |7.3 End-Cap Capacitance--Vertically suspend the test Icimens and anode in the immersion cell, observing the larances specified in 5.1.1 through 5.1.3. Fill the container Ith the electrolyte until it just covers the lower end cap.* * A material found suitable for this purpose is Baler Petroleum No. L-480-86 c Blend, Boler Petroleum Co. 85 Old Eagle School Rd., Wayne, PA J9087. where: Ka = dielectric constant, C0 = initial coating capacitance, pF, Cc = end-cap capacitance, pF, d -- outside pipe diameter, mm (in.), t0 = initial coating thickness, mm (in.), L = exposed coating length, mm (in.), and N -- 0.0556 when d, t0, L, are in mm (1.413 when d, tn, L, are in in.). 9,2 Apparent Depth of Penetration--Calculate the depth of water penetration by applying the calculated value of K0 from 9.1 and the measured value of equivalent series capacitance, C, to the following equations: 1031 DUP050298209 # G9 b ~ lo 1 t - (d/2)Ke*) - 1] where: M - NK,,L/(C - Cc), t = unpenetrated coating thickness, mm (in.), C = series capacitance, pF, and tp = depth of penetration, mm (in.). 10. Report 10.1 The report shall include the following: 10.1.1 Complete identification of specimen, including: 10.1.1.1 Name and code number of the coating, 10.1.1.2 Size of pipe, 10.1-..1.3 Source, production date, and production-run number, 10.1.1.4 Minimum, maximum, and average coating thickness, 10.1 J.5 Dates of starting and terminating test, and 10.1 .'1.6 Other information that may be pertinent, 10.1.2 Magnitude and polarity of d-c voltage applied, to sample during the test period, 10.1.3 Length of the test period in days, 10.1,4 Apparent depth of water penetration for the test period indicated, 10.1.3 Initial value of coating dissipation factor, and 10.1.6 Value of coating dissipation factor at the end ofthe test period. N' 6--For the purpose of monitoring coating performance plotted graphs of apparem depth of water penetration versus time m rectangular coordinates and coating dissipation factor versus time in. semilogarithmic coordinates will render useful information over the ' duration of the test period. 11. Precision 11.1 Due to the range of coating formulations, thick nesses, densities, etc., found among commercially available coated pipe samples; the overall accuracy and reproducibility of the test results by these methods will tend to be poorer than those expected on insulating material of a more uniform nature. 11.2 The precision (reproducibility) of the dissipation factor and depth of penetration by these methods in general is considered to be such that when two tests are performed consecutively on the same specimen under identical condi tions, the difference between the two results may normally be expected nor to exceed 5 % of their mean. The American Society for Testing and Materials fates no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users qf.thls standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are sntirely their own responsibility. ' This standard Is subject tb revision at any time by the responsible technical committee and must he reviewed every five years and ifnot revised, either teapprtmd or withdrawn. Your comments are invitedeither torrevision of this standard or for additional standards and should be addressed lo ASTM Headquarters. Your comments will receive careful consideration at a meeting of the respons/We technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee an Stahderds, ISIS Race St., Philadelphia, PA 19103. G'6i; Gil 3. Su flStfllfcP!"' 1032 ttaterfc cualii =" rigs. 1: 5.k! ' 19-mn landed 1TM IjofNonn on Dun DUP050298210 the test! Designation: G 10 - 83 (Reapproved 1988) cd 'rmancejtime in| tin>e ini 3ver the! Standard Test Method for Specific Bendability of Pipeline Coatings1 This standard is issued under the fixed designation G 10; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapproval. iScope thick, aft. 1 This method covers the specific determination of the 'ailahlpflBpct of short-radius bends on coatings applied to 33.4-mm cibifityflpn. nominal) diameter pipe. poorer P .2 This standard may involve hazardous operations and more Wmioment. This standard does not purport to address all of jfe safety problems associated with its use. It is the responsi- patinn iMijfev of whoever uses this practice to consult and establish seneral wmpropriate safety and health practices and determine the ormed applicability ofregulatory limitations prior to use. condi- sji 1.3 The values stated in SI units to three significant ally be jLcimals are to be regarded as the standard. Ri Referenced Documents I[2.1 ASTM Standards: ]5G6 Test Method' for Abrasion Resistance of Pipeline I Coatings2 j*G 12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel3 Summary of Method 3.1 The method consists of bending a 33.4-mm (1-in. ffeminal) diameter specimen of coated pipe around a manTlel to produce a range of short-radius bends. Coating failure the form of cracking or I6ss of adhesion is detected |rough visual and electrical inspection of the bent specimen. Significance and Use : 4.1 This test will provide information on the ability of Ipatings applied to pipe to resist cracking, disbonding, or Jther mechanical damage as a result of bending. Because the gist is applied to coated pipe from commercial production, fie results can be directly used in the selection of similar haterials for service. The test also has application as a |uality control method when variations in coating applica tion or material formulation will affect bending performfnce. Apparatus 5.1 The bending apparatus shall be essentially as shown in rigs. 1 to 3 and shall include the following: 5.1.1 Variable-Radius Mandrel constructed from four |l9-mm (0.75-in.) thick pieces of plywood, bolted together ind conforming to the geometric shape shown in Fig. 1. The 1 This method is under the jurisdiction ofASTM Committee G-3 on Durability bf Nonmetallic Materials and is the direct responsibility of Subcommittee G03.06 ||on Durability of Pipeline Coatings and Linings. Current edition approved May 27, 1983. Published August 1983. Originally j|i>ub!ished as G 10 - 69T. Last previous edition G 10-77. 2 Annual Book ofASTM Standards, Vols 06.01 and 14.02. geometric construction is accomplished by laying out along the outer edge of the mandrel a series of seven consecutive arcs at decreasing radii of 610, 530, 460, 380, 300, and 230 mm (24,21, 18, 15, 12, and 9 in.). The first five arcs shall be carried through a 45-deg angle to the next point of tangency. A 45-deg V-notch shall be cut into the edge of the mandrel for seating the pipe specimen. Holes shall be drilled at appropriate locations in the mandrel face for positioning the lever arm and fastening pipe clamps. 5.1.2 Lever Arm-Roller Assembly--A 1.83-rn (72-in.) lever arm with nylpn roller supplies the mechanical advan tage necessary to bend the pipe specimen. The lever arm shall contain a series of holes which are used to maintain proper clearance between the roller and pipe sample during the bending operation. 5.2 Thickness Gage--Measurements of coating thickness will be required for this test. This shall be done in accordance with Method G 12. 5.3 Holiday Detector--A low-voltage d-c holiday detector of the wet-sponge type, specified in Method G 6, shall be used to locate breaks in the coating film. 6. Test Specimens 6.1 The test specimen should be 2.5 m (100 in.) in length. It should be representative of production-coated pipe and be free of obvious coating flaws or defects. Coating specimens shall be apiplied to 33.4-mm (1-in. nominal) diameter pipe. 7. Conditioning 7.1 The specimen shall be exposed to room temperature for a sufficient time to ensure thermal equilibrium in the pipe and coating. A temperature in the range from 20 to 30C (68 to 85F) shall be considered room temperature. 8. Procedure 8.! Perform the test at a room temperature of 21 to 25C (70 to 77F). 8.2 Measure the applied coating thickness of each spec imen in accordance with Test Method G 12. 8.3 Place the conditioned test specimen into the V-notch. Secure the pipe in place with clamp No. 1 and tighten the thumb screw. Remove the threaded handle from clamp No. 1 to allow for clearance of the lever arm. With the steel pivot pin at hole A of the lever arm (see Fig. 3), insert the pin into the socket on the bed of the bending jig. Place the nylon roller at position C on the lever arm. Apply the roller to the pipe specimen, and with a constant, even force with the lever handle, bend the pipe aound the mandrel until the 460-mm (18-in.) radius bend has been made. Insert and secure pipe damp No. 2. Continue bending the pipe until the 300-mm (12-in.) radius has been reached. Insert and secure pipe 1033 D UP O50298211 # G 10 FIG. 1 Variable-Radius Mandrel clamp No, 3. Reposition the lever arm by moving the pivot pin to the 25-mm (1-in.) diameter hole in the mandrel surface. Move the nylon roller to position B on the lever arm. Apply the roller to the pipe and complete the bending operation by forming the specimen through the 230-mm (9-in.) radius. 8.4 Examine the bent specimen wth a wet-sponge holiday detector to determine at what point, if any, cracking of the coating film occurred. Note the number, size, location, and type of cracks present. Examine the pipe specimen for any loss of coating bond caused by the bending operation. N' 1--The possibility of some coatings developing stress-induced cracks in the period following the bending operation should not be overlooked. If this is a consideration, the bent specimen should be retained for a 24-h post-bent inspection. 9. Report 9.1 The initial test report shall include the following: 9.1.1 Complete identification of the coated pipe tested, including: name and type of coating, average coating thick ness, minimum coat.ing thickness, maximum coating thick ness, manufacturer's Ipt number, and date of manufacture. 9.1.2 Temperature of the pipe specimen as tested, 9.1.3 Radius at which cracking first'Occurred, , 9.1.4 Description ofthe type of cracking, 9.1.5 Location and extent of any loss in pipe-to-coating bond, 9.1.6 Number of specimens tested, 9.1.7 Any peculiar characteristics of the specimen noted during the test or after immediate removal from the test apparatus, and 9.1.8 Post-bend retention time. 1/2 X mi LAG SCREWS WCSTO.SA5XPSMH5MaE8RtBJMO/aMTVT(OMjiM/.271E*ftXNATJf L6012M')M X 50I.2"Ml M% XStV.MlMX 25(010*1MM h* 5^'THRU BOLTS CSKJ6 MM OVj*)* X U.SMmVsVTOT ONLY LtSXaO6*i MMMM(2i'1VXl SO MM12' X2O0 L12S'Ol XUM(2M';MXSIVOVJXMM 300 MM fl2*l n 1 t, I FIG. Z Details o< Mandrel Assembly and Support Brackets 1034 f DUP050298212 # G 10 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination.of the validity of any such patent rights, .and the risk of infringement of such rights, are entirely their own responsibility. This standard Is subject to revision at any time by the responsible technics] committee and must be reviewed every fto years and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should, be addressed to ASTM Headquarters. Your comments wili receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feeI that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Bace'St., Philadelphia, PA 19103. 1035 DUP05029821 3 Designation; G 11 - 88 Standard Test Method for Effects of Outdoor Weathering on Pipeline Coatings1 This standard is issued under the fixed designation G 11; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope 1.! This test method is intended to define conditions for the exposure of coated pipe to weather. 1.2 This test method specifies qualifications for the sam ples, procedure to be followed in exposure to weather and procedure for evaluating effects of exposure including visual examination and other tests. 1.3 This test method may involve hazardous operations and equipment. This test method does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this test method to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1.4 The values stated in SI units to three significant decimals are to be regarded as the standard. the longer the exposure period, the more reliable are ih results obtained. 4. Summary of Test Method 4.1 The effects of outdoor weathering on pipeline coating after 6,12, and 24 months' exposure are determined visual! t and by electrical means by comparing exposed samples ot coated pipe with unexposed samples of coated pipe befo.j and after impact and bending tests. At the beginning of Hi test the starting^ samples are qualified by a cathodic disbonding test. p. Location of Test Sites , 5.1 Weathering racks shall be located in cleared ana-, representative of local outdoor weather Conditions. 2. Referenced Documents 2.1 ASTM Standards: G 8 Test Methods for Cathodic Disbonding of Pipeline' Coatings2 G 10 Test Method for Specific Bendability of Pipeline Coatings2 G 12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel2 G13 Test Method for Impact Resistance of Pipeline Coatings (Limestone Drop Test)2 G62 Test Methods for Holiday Detection in Pipeline Coatings3 G70 Test Method for Ring Bendability of Pipeline Coat ings (Squeeze Test)3 3. Significance and Use 3.1 Since coated pipe may be stored outdoors for long periods before burial, weathering tests of the type described in this test method are needed to evaluate the stability of these coatings stored outdoors. The results obtained should be treated only as indicating the general effect of weathering. Exposure conditions vary greatly from year to year, from one part of a year to another, and from locality to locality. The results of short-term exposure tests in the north are more meaningful if exposure is started in the summer followed by . a winter season. In southern areas where climatic conditions are more uniform throughout the year, the time of year when short-term exposure is started is less critical. In all localities, 1 This test method is under the jurisdiction of ASTM Committee G-3 on Durability of Nonmetallic Materials and is the direct responsibility of Subcom mittee G03.06 on Durability of Pipeline Coatings and Linings. Current edition approved May 27, 1988. Published July 1988. Originally published as G 11 - <59 T. Last previous edition G 11 - 83. 2 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 3 Annual Book ofASTM Standards, Vol 14.02. 6. Apparatus 6.1 Racks--The horizontal racks shall be any suitable pipe storage racks of sufficient height to'prevent any unde sirable effects of vegetation growth during the period exposure. Racks may be constructed from a variety materials, but pipe specimens must rest on a nonconductive* surface. An example of a suitable rack is illustrated in Fig, It 7. Sampling 7.1 Each starting sample shall consist of coated 26.7-mm,, (34-in. nominal) diameter steel pipe from a production lbf having a minimum length of 4.4 m (14.4 ft). The sample shall be from a lot produced under conditions capable of being duplicated on a production scale. N' 2--Pipe having a nominal diameter of 33.4-mm (I-in. nom-,* inal) can be used and is the largest diameter that can be evStualed ;u accordance with Test MethocLG 10. Larger diameter pipes can be evaluated in accordance with Test Method G 70. 7.2 Each starting sample shall have a piece 600-mn. (24-in.) long cut from one end by sawing for use in qualification testing (Section 8) and designated the "qualifi cation sample." The remainder of each starting sample shall be designated the "sample." 7.3 The total number of samples for each coating in test shall be four, divided as follows: 7.3.1 One to be removed after 6 months exposure, 7.3.2 One to be removed after 12 months exposure, 7.3.3 One to be removed after 24 months exposure, and 7.3.4 One to be used for determining original contro. values, which should be obtained as soon as possible on receipt of the pipe. 8. Procedure for Qualification Testing 8.1 Test each qualification sample in accordance with Test Methods G 8, Method B. 1036 pisK . t 8.2 | he Mi 8.3 ' eeisi nplef ,'8.'4 ( pr4- M u { mAabop 3- | th TrI., 9.4 | ;or,|t-:: 9.5 if' ating: atelyntini. her L posit;gthR: si lllllilii st.-.rs DUP050298214 G 11 gAII lumber is to be pretrealed and painted. FIG. 1 Construction Details of Outdoor Weathering Rack Begin qualification testing at the same approximate ample testing. fthe results of the qualification testing are within the limits given in Test Methods G 8, consider the Mo be reasonably equivalent and proceed with testing. fthe results of the qualification testing are not within lision limits given in Test Methods G 8, consider the Spio be unequivalent and discontinue exposure testing. ? edure for Sample Testing jpentify the test samples with a letter, number, or for ready identification after exposure. The marking interfere with either the exposure or the testing, tote and record the appearance of the sample, ieasure and record coating thickness in accordance Method G 12. 'heck coating for holidays with the appropriate de- described in Test Methods G 62. ake two 80-mm (3-in.) long scribes through the jto bare metal. Begin one scribe at a point approxi230 mm (9-in.) from one end of the pipe and je it for 80-mm along the length of the pipe; begin the Iribe at a point approximately 230-mm from the end of the pipe and continue it for 80-mm along the the pipe. One scribe should be on the top of the other on the bottom. tount the samples on the rack as shown in Fig. 1 with facing skyward and one facing toward the ground, [he three samples together so that like samples are gside one another, liter exposure, again note and record the appearance Imple and check for holidays in the manner followed prior to exposure. Next examine the sample visually for cracking, checking, blistering, corrosion, undercutting from the intentional scribe, and any other form of impairment of the coating. 9.8 Finally, cut a 300-mm (12-in.) specimen from one end of the sample, where the scribe is facing downward, and subject to an impact test in accordance with Test Method G 13. In the impact test, position the specimen so that the scribe faces downward. 9.9 Subject the remaining 2.5 m (8.2 ft) to a bend test in accordance with Test Method G 10. In the bend test, position the skyward face of the sample as the outside of the bend. 9.10 Follow the procedure in 9.7, 9.8, and 9.9 on samples removed after each of the three exposure periods and compare results with those obtained on the control sample in 7.3. 10. Report 10.1 The report shall include the following: 10. t -1 Results of qualification tests, 10.1.2 Sample number and description of coating system including: surface preparation, method of application, and coating thickness, 10.1.3 Appearance of sample and presence or absence of holidays prior to exposure, 10.1.4 Appearance of sample, presence, or absence of holidays after exposure, and duration of exposure, 10.1.5 Visual evidence of coating failure as noted by 9.7, 10.1.6 Results of impact and bend tests after exposure as compared with those for the control sample, and 1037 DUP050298215 ft G 11 10.1.7 Type of environment and exposure. 11. Precision 1J.1 The precision requirements for qualification testing in Section 8.3 of this test method and the precision requirements given in Test Method G 12 shall apply. Variations hi samples and qualification samples shall be within respective precision limits for this test method to be valid. 1$ The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, eitherreapproved or withdrawn. Your comments are invitedeither for revision of this standard or lor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting pf the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your Wews known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. IScopd i.i Tit. emeni Splied tj |omme ijkfor^ % It d| j|.2 4 lof the/ sporislli ijjproprfk iMicabtt , ! 1.3 m <icimalsi Sumnf |2.1 Tlj.' hat mea| variaf -- yeen its; . Sigitif: 3.1 ii - |fmost A |dequat< unction : pipelines/: 3.2 Tlv nfluertcA' ' nethod ' JefornjaK measurir|',r~ . Appall:.4.1 Tl| ness gage. |ntendedp> j.|nagneti<f Sinit anc$A Ihicknes'" 4.2 It I' Inonmagifc 1038 1 This :Durabilily || ]1 i'mittec G3.C Current i ^published ag* DUP050298216 1ID Designation: G 12 - 83 (Reapproved 1988) uirens in ctive Standard Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel1 This standard is issued under the fixed designation G 12; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval. 1 Scope 1.1 This test method describes the nondestructive meaJtrement of the thickness of a dry, nonmagnetic coating fclied to the external surface of steel pipe. The method is ^commended for coating thicknesses up to 6 mm (0.240 in.) ad for any diameter pipe, but not smaller than 10 mra (0.5 |i.). It does not apply to excessively soft films. |' l.2;r7Ms test method may involve hazardous operations nd equipment. This test method does not purport to address Mil of the safety problems associated with its use. It is the Responsibility of the user of this test method to establish Appropriate safety and heath practices and determine the applicability ofregulatory limitations prior to me. I 1.3 The values stated in SI units to three significant decimals are to be regarded as the standard. Summary of Test Method r 2.1 The coating thickness is determined by an instrument Jjhat measures thickness by nondestructive techniques, based ISm variations in magnetic flux or magnetic attraction be tween its detection unit and the magnetic base material. . Significance and Use 3.1 Measurements of film thickness are an essential part gbfmost ASTM test methods related to coatings on steel pipe, j&dequate thickness is important for a coating to fulfill its Junction of preventing or mitigating corrosion of steel (pipelines. 3.2 The accuracy of the thickness measurements may be ^influenced by the deformability of the coating. This test aethod is not applicable to coatings that would be readily peformable under the force exerted by the probe of the neasuring instrument. |4, Apparatus 4.1 The apparatus shall be a nondestructive-type thickBness gage capable of being standardized over its range of intended use. It shall be designed so that variations in fmagnetic flux or magnetic attraction between its detection (unit and the steel base can be calibrated to indicate the thickness of the coating material. 4.2 It shall be suitable for measuring thicknesses of dry, 1 nonmagnetic coatings on either a flat or a circular base. 1 This test method is under the jurisdiction of ASTM Committee G-3 on \ Durability of Nonmetallic Materials and is the direct responsibility of Subcom| mittee G3.06 on Durability of Pipeline Coatings and Linings. Current edition approved June 24, 1983. Published August 1983. Originally published as O 12 -69 T. Last previous edition G 12 - 77. 5. Standardization of Instruments 5.1 The instrument shall be standardized m accordance with the manufacturer's instructions before use by em ploying suitable thickness standards. The standardization shall be checked at frequent intervals during use. 5.2 Nonmagnetic standards of uniform thickness are available in either of two types, foil or coated substrate, as supplied or recommended by the manufacturer of the instrument. 5.2.1 Foils (Shims)--The thickness ofthe foil should be as close as possible to the expected thickness ofthe coating to be measured. The foil should be placed on a smooth, clean, low-carbon, steel plate, making certain that there is intimate contact between the foil and the substrate. 'It is recoriimended that single foils of proper thickness be used and that foils be replaced frequently, since they are subject to inden tation. Foils are advantageous for standardizing oh curved surfaces and are often more readily available than coated standards. N' 1--For some instruments there is an effective depth of penetration of the field created by the instrument probe. This is the critical depth of thickness at which the instrument wili no longer be affected by increases of substrate thickness. Since it depends on the instrument and substrate, it should be determined experimentally. 5.2.2 Coated Substrate Standards2--These standards con sist of nonmagnetic coatings of known thickness perma nently bonded to a iow-carbon steel (1010 grade) substrate, 8 mm (0.30 in.) thick. The thickness standard should be as close as possible to the expected thickness ofthe coating to be measured. N' 2--If the curvature of the coating to be measured is sufficient to preclude standardization on a flat surface, the standardization should be done with a standard foil on a substrate with the same curvature as the coating to be measured. 6. Procedure 6.1 Operate each instrument in accordance with manufacturer's instructions. 6.2 Take a minimum of twelve readings per piece of pipe as follows: Take three equally spaced readings along the top surface; rotate the pipe 90 three times, taking three equally 2 Coated substrate standards may be obtained from the U. S. Department of Commerce, National Bureau of Standards, Standard Materials Unit, Washington. DC 20234. 1039 DUP050298217 # <3 12 81 spaced readings after each rotation. Record the average, minimum, and maximum of the twelve readings as the coating thickness. N' 3--Instruments with two contact poles shall be positioned on the coating surface with the poles in the same plane. N' 4--The anchor pattern of the steel pipe substrate must be considered for its effect on the accuracy of the measurements if the anchor pattern is greater than '25 % of-the coatihg thickness. N' 5--Foreign materials such as dirt and grease shall be removed by suitable cleaning without removing any coating materials. N' 6--Measuring instruments and methods may depend on the technique of the operator. For example, the pressure applied to a probe and the rate of applyitiga balancing force to a magnet will vary from one individual to another. Often such differences can be reduced or eliminated either by having the gage calibrated by the same operator who will make the measurement or by using constant-pressure probes. Probes must be positioned perpendicular to the surface of the specimen at the point of measurement. Some magnetic ipstrunjents of the magnetic-attraction type require the pole piece to be in a vertical position. If a magnetic instrument is to.'be used in a horizontal or upside-down position, its calibration for that position should'be verified. N' 7--Instruments using magnetic attraction are sensitive to the speed with which the magnet is removed from the specimen. The magnet must be removed so. that thickness measurements are not affected by speed of removal. 7. Report 7.1 The report shall include the following: 7.1.1 Complete identification of the specimen including- name and code number of the coating; pipe diameter- source; production data, including surface preparation o-'t'h - substrate and depth of anchor pattern, if known; mj production run number. 7.1.2 Name and type of instrument used, and method of standardization, and 7.1.3 Number of thickness measurements taken, and the average, minimum, and maximum value of the measure ments. .. . .' 8. Precision- 8.1 The repeatability and reproducibility of thickness measurements wili depend on thb instrument design, the operator,1 and the particular measuring application. 8.1.1 Repeatability--When the same instrument is used by the same operator, duplicate measurements on the Same sample should agree with each other within 5 %. 8.1.2 Reproducibility--Separate operators using different instruments on a known thickness standard should obtain average results agreeing with' each other within 10 % of the thickness standard. Tha American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection ' with any item mentioned In this standard. Users of this standard are expressly advised that determination ofthe validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. , , This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are Invited either for revision of this standard or foradditional standards arid should be addressed lo`ASTM Headquarters, your comments witl receive careful consideration at a meeting of the responsible technical committee, which you may attend. It you feel that your comments have nof received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103% Re|,. 1040 ; Appari . 5.1 Thfr/- 1 ant#; 5.U 1 This test* ability off e G03.p| Orient eq ished as < f Annual 1 * Annual B, l* DUP050298218 Designation: G 13 - 89 mg: Standard Test Method for iter, Impact Resistance of Pipeline Coatings 'the and (Limestone Drop Test)1 i of the ure- tiess" thfe- irae rent taiif the This standard *is Issued under the fixed designation G 13; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval, A superscript epsilon () indicates an editorial change since the last revirion or reapproval. I Scope 1,1 This test method covers the determination of the lative resistance of pipeline coatings to impact by observing ge effects of falling stones on coated pipe specimens. 11.2 This standard may involve hazardous operations and mtipment. This standard does not purport to address all of We safety problems associated with its use. It is the responsiIiity of the user of this standard to establish appropriate mfety and health practices and determine the applicability of spdatory Imitations prior to use. 71.3 The values stated in SI units are to be regarded as the andard. stones from a height of 1830 mm (6.0 ft) measured to the top of a piece of coated pipe under test. Construction details are shown in Fig. 2. N' I--The box and ohute described in Fig. 2 are designed for testing coatings on lQO-mm (4-in.) and 150-mm (6-in.) pipe specimens. Smaller diameter pipe may be used by inserting wood V-blocks in the trough in the box below the chute. 5.1.2 Stones, hard, coarse, limestone aggregate, con forming to AASHTO Designation: M80-51 (No. 67) which is taken from American Association of State Highway and Transportation Officials "Standard Specifications for Coarse Aggregate for Portland Cement Concrete." Referenced Documents 2.1 ASTM Standards: G12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel2 G62 Test Methods for Holiday Detection in Pipeline Coatings3 ' . | 2.2 AASfTO Standard: M80-51 (too. 67) Specification for Coarse Aggregate for Portland Cement Concrete & umniary ofTest Method ' 3.1 The impact resistance of pipeline coatings is deter- gmined by dropping weighed amounts of a specified type of limestone through a chute onto a coated pipe specimen. Results are reported as the number of drops required to Bbierce through the coating to bare metal, as determined visually or electrically. in N' 2--These specifications cover the quality and size of coarse aggregate. No. 67 designates a 19-mtn <5/4-in.) to No. 4 size stone with the following sieve analysis: Square Opening, mm (in.) Weight % Passing 25(1) 19 ('/<) 10 04) No. 4 100 95 to 100 20 to 55 0 to 10 5.1.3 Bucket--Any suitable bucket that will hold 16 kg (35 lb) of stones. 5.1.4 Holiday Detectors--Two types are needed as de scribed in Test Method G 62. N' 3--A holiday is defined as small faults or pinholes that permit current drainage through protective coatings on steel pipe. 5.1.5 Thickness Gages--Any instruments suitable for use with Test Method G 12. 6. Test Specimens significance and Use 4.1 This'test Is intended to simulate the effects of ackfilling after pipe has been placed in the trench. The ackfill is often rocky soil and, if it is unscreened and the oated pipe is unshielded by sand or other protective adding, the falling rocks may seriously damage the coating. . Apparatus 5.1 The impact apparatus shall be essentially as shown in rig, 1 and shall include the following: 5.1.1 Box with Chute, providing a means of dropping 6.1 Test specimens shall be 600 mm (24 in.) Icing and shall be cut from a representative piece of coated pipe. Only holiday-free specimens shall be used in the test. 7. Procedure 7.1 Perform the test at a room temperature of 21 to 25"C (70 to 77F). .7.2 The procedure consists of dropping up to 10 buckets of stones on coated specimens. The number of buckets of stones required represents the resistance of the coating to this type of impact. 7.3 Place the test.specimen in the trough below the chute. 1 This test method is under the jurisdiction of ASTM Committee G-3 on Durability of Nonmetallic Materials and is the direct responsibility of Subcomnittee G03.06 on Durability of Pipeline Coatings and Linings, Current edition approved'April 28, 1989. Published June 1989. Originally 'ublished as G 13 - 69 T. Last previous edition G 13 - 85: 3 Annual Book ofASTM Standards, Vols 06.01 and 14.02. 3 Annual Book ofASTM Standards, Vol 14.02. Insert the retaining board in the top part of the chute and hold it in place across the chute opening with a suitable metal or wood clip. Weigh 16 0.2 kg (35 0.5 lb) of stones into the bucket. Lift the bucket to the top of the chute. Empty the stones into the trough formed by the hopper walls and the retaining board so that the stones are distributed evenly in the trough. Detach the holding clip from the 1041 i: DUP050298219 # G 13 FIG. 1 Box, Chute, and Bucket FIG. 2 Construction Details of Box and Chute retaining board and tilt the board forward to release the stones. Experience with this procedure has indicated that the stones are so constricted within the narrow confines of the chute that they fall in a uniform manner. 7.4 After each drop, remove the specimen. Examine the specimen visually for breaks in the coating. If there are ho visual breaks, check with the holiday detector appropriate for the coating thickness for holidays in the coating. If there is no visual or electrical evidence of holidays, repeat the test until the first holiday is detected and record the number of drops and the number of holidays detected. In repeating the test, the specimen should be replaced in the trough so that the same portion of the coated surface is always subjected to the falling stones. After the Same stones have been used five times, they should be replaced. 7.5 If no failure has occurred after 10 buckets, terminate the test. N' 4--As indicated in 7.4, the same charge of stones may be used five times. Experiments in which the same charges- of stones were dropped more than five times have shown relatively little attrition of the stones. ' ' 8. Report 8.1 The report shall include the foilowing: 8.1.1 Complete identification of the specimen including:name and code number of the coating, pipe diameter, coating thickness, source, production data, and productionrun number, 8.1.2 Approximate pipe temperature at the beginning and at the end of the test, and 8.1.3 Number of buckets of stone,to produce the first-; holiday and the number of holidays produced during this drop. N' 5--If there is a large number of holidays after a given number of drops, the report should state this by the term "too numerous to count11 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision atany time by the responsible technical committee end must be reviewed every five years and if not revised, either reapprovedor withdrawn. Your comments are invited either for revision of this standard or tor additional standards and should be addressed to A&TM Headquarters. Your comments will receive careful consideration at a moating of the responsible. technical committee, which you may attend. If you feel that your comments have not received a fa/r hearingyou should make your views known to the ASTM Committee on Standards, 1916 Race $t, Philadelphia, PA 19103. is. Ap. 5.lti Vippai|; 1042 DUP050298220 Designation: G 14 - 88 Standard Test Method for Impact Resistance of Pipeline Coatings (Failing Weight Test)1 This standard is issued under the fixed designation G 14; the number immediately following the designation indicates the year of . original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (0 indicates an editorial change since the last revision or reapprovaJ. [F i' LScope Mil This test method covers the determination of the ftergy required to rupture coatings applied to pipe under ecified conditions of impact from a falling weight. 1.2 This test method may involve hazardous operations W equipment. This test method does not purport to address ttl of the safety problems associated with its use. It is the msponsibility of the user.of this test method to establish Jppropriate safety and health practices and determine the fppliiability ofregulatory Imitations prior to use. 1.3 The values stated in SI units to three significant ijecimals are to be regarded as the standard. |. Referenced Documents 2.1 ASTM Standards: G 12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel2 G62 Test Methods for Holiday Detection in Pipeline Coatings3, 2.2 SAE Standard: Grade 52100 Steel4 e used i were ofthe" tdingjj neter, ;tiongand K)-, Summary of Test Method A ^S i A 3.1 This test method uses a falling fixed weight having a fipecified diameter impact surface, tup, which is restrained Vertically and dropped from varying heights to produce i'jmpaet energies over the required range. Electrical inspection Is used to detect resultant breaks in the coating. Impact resistance is determined as the amount of energy required to Irause penetration of the coating film. p. Significance and Use j 4.1 The ability of a pipe coating to resist mechanical ^damage during shipping, handling, and installation will '(depend upon its impact resistance. This test method provides a systematic means for screening coating materials with regard to this property. 5. Apparatus 5.1 This test method can be successfully used with impact apparatus conforming to the following specifications: 1 This test method is under the jurisdiction of ASTM Committee G-3 on Durability of Nonmetallic Materials and is the direct responsibility of Subcom* mittee G03.06 on Durability of Pipeline Coatings and Linings. Current edition approved May 27, 1988. Published July 1988. Originally published as G 14 - 69 T. Last previous edition G 14 - 83. 7 Annua! Book ofASTM Standards, Vols 06.01 and 14.02. 3 Annua! Book ofASTM Standards, Vol 14.02. 4 Available from Society of Automotive Engineers, 400 Commonwealth Drive, Warrendale, PA 15096. 5.1.1 Tup--The tup shall be made up from a tup body and a tup nose having a combined, fixed weight of 1.361 kg (3.00 lb) and shall be used over a drop range of 0.61 to 1.22 m.(2 to 4 ft). With most coatings, a 1.361-kg (3.00-lb) tup dropped through a distance of 914 mm (3 ft) yields suitable results. The tup nose shall have a 15.875-mm (Vs-in.) hemispherical head. N' 1 --Frequent replacement of the tup nose can be avoided if it is cut from steel capable of being hardened to a hardness of Rockwell C/45 while retaining an impact toughness of at least 15 ft-lb (20.34 J). Ball bearings conforming to SAE Grade 52100 have also been found suitable for this purpose. 5.1.2 Drop Tube--A tube 1.52 m (5 ft) long shall be used to contain the tup and guide it during free fall The drop tube shall be constructed of steel, aluminum, or any other suitably rigid material and internally sized to provide a minimum of friction to the falling tup. A scale shall be attached for measuring the height of drop to the nearest 2.54 mm (0.10 in.). 5.1.3 Specimen Holder--The base plate of the apparatus shall include a device for positioning and holding the pipe specimen on line with the axis of the vertical drop tube. N' 2--An arrangement using a V-notch vise made .of metal with spring clamp is recommended for this purpose. Glancing blows, caused by an out-of-plumb condition between drop tube and pipe sample, will cause erratic test results. 5.1.4 Apparatus Support---Both the apparatus and sample shall be firmly supported and secured to a rigid base to optimize energy transfer from the tup to the specimen. 5.2 A design for the test apparatus appears in'Figs. Xl.l through X 1.3 of Appendix XI. 5.3 Thickness Gage--Measurements of coating- thickness will be required for this test, and shall be done in accordance with Method G 12. 5.4 Holiday Detector--A suitable detector as specified in Test Methods G 62 shall be used to locate breaks in the coating film. 6. Test Specimen 6.1 The test specimen shall be a 406.4 mm (16 in.) long piece of Schedule 40, 60.325 mm (2.375 in.) outside diam eter coated pipe prepared with its surface preparation and coating procedures equivalent to that of production coated pipe. 6.2 Seven specimens shall be required for the test. 7. Conditioning 7.1 The specimen shall be exposed to a room temperature of 21 to 25C (70 to 77F) for a period of 24 h before beginning the test. 1043 DUP050298221 # G 14 8. Preliminary Measurements 8.1 Measure the applied coating thickness of each spec imen in accordance with Test Method G 12. 8.2 Place test specimen in sample holder and lightly place tup on surface of the coating. Adjust either the drop tube or the attached scale so that the wing bolt (lifting pin) is at the zero mark of the scale. 8.3 Make a preliminary set of impact readings to deter mine the approximate starting point for the test. This shall be done by strildng the first specimen from a height sufficient to cause failure of the coating film. Consider any penetration a failure if it is detectable with a suitable Holiday Detector as specified in Test Methods G 62. '8.3.1 Reduce the height by 50% and make a second exploratory drop at a fresh area on the pipe surface. Continue testing in this manner, with the corresponding reduction in height between drops, until the coating fails to break. No t ' 3--Choose test locations at the specimen surface in a random manner and keep at least a 76.2-mm (3-in.) distance between adjacent points of impact and within 38 mm f 1 Vi] in.) from the ends. Choosing test points in any regular pattern will bias the experiment and introduce error into the test results. 8.3.2 Repeat the test at the height immediately preceding the occurrence of the nonfailure to determine if an approxi mate level for the mean impact strength has been bracketed. Two successive reversals of coating performance between failure and nonfailure will give sufficient indication that the point has been reached. 9. Procedure 9.1 Perform the test at a room temperature of 21 to 25C (70 to 77F). 9.2 Begin testing from the approximate height determined in 8.2 and corresponding to the point at which the first nonfailure was registered. Maintain a fixed increment be tween adjacent testing heights. 9.3 Use a suitable detector, as specified in Test Method G 6, to determine penetration or lack thereof of the coating after ea'ch individual impact. 9.4 If the coating film is penetrated on the initial drop, make the next test at the next lower height increment. If the first specimen does not fail, make the second test at the next higher increment. 9.5 In a similar manner, determine the height of fall by the performance of the coating on each preceding drop. Maintain a constant height increment between readings. Continue to apply this "up-and-down" method4 until 20 successive impact readings have been made. 4 This system of testing, nomenclature, and calculation is described by Dixon, W, J. and Mood, A. M., nA Method for Obtaining and Analyzing Sensitivity Data," Journal Am. Statistical Assn., JSTNA, Voi 43, March, 1948, p. 309. 10. Calculation 10.1 Calculate the mean value of impact strength, m, in g/cm (or in./lb) as follows: where: ha = minimum height at which the less frequent event occurs, cm (or in.), d = increment in height of drop, cm (or in.), A = sum of the frequency of occurrence at each height increment times the number of increments above the k0 value for each observation itrthe N total, N = total number of the less frequent- event (coating failures or nonfailures), and W = tup weight, g (or lb). NOTE 4--The minus sign is used when the calculation of the mean is based on the total number ofcoating failures and the plus sign when it is based on the nonfailures. 10.2 Calculate the sample standard deviation, s, in gramcentimetres (or inch-pounds) as follows: 5 = 1.620 dW+ cj where: C = 0.737 when d is in cm, or 0.029 when d is in in., d, N, A, and W are as defined in 10.1, and B = sum of the frequency of occurrence at each height increment times the square of the number of incre ments above the h0 value for each observation in the N total. N' 5--Adequate definition of coating impact strength will result only if the height increment, d, has been properly chosen. When testing polymeric films in the range front 0.254 to 1.016 mm (0.010 to 0.040 in.), height increments of from 5.1 to 12.7 mm (0.2 to 0.5 in.) have been found suitable with the 1.361-kg (3.0-lb) tup. Larger increments may be necessary for thicker materials. If after making tfre calculations of 10.1 and 10.2, the ratio of the height increment to the standard deviation (d/s) is less than 0.20, the test should be repeated using a larger value for the increment d. This procedure will result in an improved estimate of the coating impact strength. 10.3 An illustration of the use of these equations appears in Appendix X2. ----- II. Report 11.1 The report shall include the following:, 11.1.1 Complete identification of the specimen including: 11.1.1.1 Name and code number of the coating, 11.1.1.2 Size of pipe, 11.1.1.3 Source, production date, and production-run number, 11.1.1.4 Minimum, maximum, and average coating thickness, 11.1.1.5 Date of test, and 11.1.1.6 Other information that may be pertinent, 11.1.2 Average impact strength in g/cm (or in./lb), 11.1.3 Sample standard deviation in g/cm (or in./lb). t! ! r * ; I it 1044 DUP050298222 <> G 14 . in APPENDIXES (Nonmandatory Information) XI. SUGGESTED DESIGN FOR TEST APPARATUS 'ent 1.1 A design for the impact test apparatus is shown in Figs. Xl.l to XI.3. Ight the ''3 Una an is lit fs am- ght trethe esult sting 1.040 been ty be 10.1 ition ie for ite of ai>. ling. k -run tting . 1045 DUP050298223 # G 14 (8 /j.l!H W Z 9 i1V - j . f'1-- l,,Z )H W 0 8 '0 5 FIG. X1.3 Detailed Design o( Test Apparatus 1046 DUP050298224 G 14 X2. SAMPLE CALCULATIONS K2.1 Test results for 20 drops with a 1,361-kg (3-lb) tup are given in Table X2.1. TABLE X2.1 Test Results Test No. Height of Drop, in. Failed Test No. Height of Drop, in. Failed 1 14.1 yes 2 13.8 no 3 14.1 no 4 14.4 yes 5 14.1 yes 6 13.8 no 7 14.1 no 8 14,4 yes 9 14.1 yes 10 13.8 yes 11 13.5 no 12 13.8 no 13 14.1 yes 14 13.8 yes 15 13.5 no 16 13.8 yes 17 13.5 yes 18 13.2 no 19 13.5 no 20 13.8 yes Height increment 0.3 in. Failures -= 11 Nonfailures = 9 Nonfailures at 13.2 in. (h,,) = 1; at 13.5 In. = 3; at 13.8 In. = 3; at 14.1 in. = 2 A = (0 X 1) + (1 X 3) + (2 X 3) + (3 x 2) = 15 B = ((0)2 x 1) + <(1)2 x 3) + 2)2 X 3) + 3)2 x 2) = 33 m = [l3.2 + 0.3 (~^ + g)] 3.0 - 41.55 in. -lb mean impact resistance >* 41.55 i.-lb S = 1.620 x 0.29 x 3.0 (-- ^ = 1.338 In.-lbs. Sample standard deviation 1.383 in.*lb - The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection withany item mentioned in this standard, users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standardis subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invitedeither forrevision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, whtch you may attend, if you feel that your comments have not received a telr hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. ;\ 1047 DUP050298225 Designation: G 17 - 88 Standard Test Method for Penetration Resistance of Pipeline Coatings (Blunt Rod)1 This standard is issued under the fixed designation G 17; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapprovai. A superscript epsilon (0 indicates an editorial change since the last revision or reapprovai. 1. Scope 1.1 This accelerated test method is used to determine the relative resistance of steel pipeline coatings to penetration or deformation by a blunt rod under a specified load. The test method is intended to apply to the testing of all types of nonmetallic pipeline coatings subjected to various tempera tures. 1.2 This test method may involve hazardous operations and equipment. This test method does not purport to address all of tfte safety problems associated with its use. It is the responsibility of the user of this test method to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1.3 The values stated in SI units to three significant decimals are to be regarded as the standard. 2. Summary of Test Method 2.1 The depth or rate of penetration or deformation that is caused by a weighted blunt rod to a coating system applied to steel pipe is measured over a period of time with a micrometer depth gage. Three consecutive identical readings taken at specified intervals conclude the test. 3. Significance and Use 3.1 Since pipeline coatings are subjected to concentrated pressures exerted by the weight of the pipe and the backfill, this test is intended primarily for determining the resistance of the coating to penetration or deformation under con trolled conditions. 3.1.1 Deformation of a compressible coating does not signify a.potential weakness in underground burial service, if .the coating is not penetrated. Deformation cannot be com pared to penetration into and through a coating. 4. Apparatus 4.1 Test apparatus shall consist of a dead weight tester that can press the flat tip of a rod against the coated pipe. The flat-tipped end of the rod contacting the coating shall have a diameter of 6.350 mm 0.0254 mm (0.250 in. 0.001 in.) and together with supplementary weight and any other weight-contributing parts shall have a total weight of 4.453 kg (9.817 lb), resulting in a unit pressure of 14.060 1 This test method is under the jurisdiction of ASTM Committee G-3 on Durability of Nonmetallic Materials and is the direct responsibility of Subcom mittee G03.06 on the Durability of Pipeline Coatings and Linings. Current edition approved May 27, 198$. Published July 1988. Originally published as G 17 - 71 T. Last previous edition G 17- 83C1. FIG. 1 Blunt Rod Penetration Tester kg/cm2 (200 pri) against the coating. Detailed design of the apparatus is shown in Fig. i through 6. 4.2 Depth Gage, a device capable of measuring the penetration movement of the rod accurately to 0.0254 mm (0.001 in.). 4.3 Temperature Chamber, a thermostatically controlled enclosure to provide heating and cooling of the specimen and test apparatus (excluding depth gage) to within 2'C (3.6F) of the desired test temperature. This equipment is optional when the test can be run within 2C (3.6F) of the desired test temperature without its use. 4.4 Temperature Controlled Box, to fully enclose the test apparatus except the indicating means of the depth gage, as optional equipment in cases where a test is to be run at a temperature higher than room temperature. The enclosure shall be thermostatically controlled, capable of maintaining the temperature to within 2C (3.6F) of the test tempera ture, which normally will be in the range of 23 to 76.6"C (73.4 to 170F). 4.5 Thermometer, a temperature measurement device accurate to 0.5C (1F). 5. Test Specimens 5.1 The test specimens shall be 150 mm (6 in.) long and prepared with its surface preparation and coating procedures 1048 ti DUP050298226 # G 17 H Symbol if A S'; B Wc V D rb "F G I' H 8i .J rK r. G ' M 1N *0 P 1 1 RQ |S 1T |u TABLE 1 Dimensions for Fig. 3 mm 1.59 3.18 7.94 8.73 9.53 10.32 12.70 15.86 19.05 20.64 25.40 38.10 55.56 63.50 76.20 111.13 127.00 184.15 215.90 50.80 88.90 in. 0.063 0.125 0.313 0.343 0.375 0.406 0.500 0.625 0.750 0.813 1.000 1.500 2.188 2.500 3.000 4.375 5.000 7.250 8.500 2.000 3.500 Symbol A B C D E F G H 1 J K L M N O P Q R S T U V w TABLE 2 Dimensions for Fig. 4 mm 0.79 1.59 3.99 mu 12.70 12.70 12.71 12.72 13.49 14,29 15.88 17.46 19.05 19.08 25.40 3B.10 60.33 92.08 101.60 120.65 141.29 184.15 203.20 in. 0.031 0.063 0.157 0.438 0.500 0.500 0.500 0.501 0.531 0.563 0.625 0.688 0.750 0.751 1.000 1.500 2.375 3.625 4.000 4.750 5.563 7.250 8.000 fell be run. Conditioning jfc.l The specimen shall be exposed to the test temperature |r a period of 24 h before beginning the test. If the test fpiperature is the same as room temperature, it shall be 21 i 25C (70 to 77F). 7. Procedure 7.1 Perform the test at room temperature or at the selected temperature. 7.2 Accurately measure the thickness coating in the area to be tested. Assemble the sample and end plates. Position the sample in the test unit so that the known film thickness DUP050298227 G 17 Symbol A B c D E F G H 1 J K L" M N O TABLE 3 Dimensions for Fig. 5 mm 1.59 6.35 6.35 9.50 9.53 9.55 10.32 19.05 19.06 19.07 25.40 64.29 63.50 101.60 165.10 . - in. 0,063 0.260 0.250 0.374 0.375 0.376 0.406 0.750 0.750 0.751 1.000 2.531 2.500 4.000 6.500 area is directly under the weighted rod and hold the sample in position by use of the cap screws. 7.3 Loosen the shaft collar and allow the weight to rest on the shaft guide. Using the depth gage take a measurement without the load applied. Raise the weight and tighten the set screw in the collar so that the weight rests on the shaft. 7.4 Take measurements every 24 h. 7.5 Continue the test until the maximum penetration has been reached as evidenced by three consecutive unchanged measurements. 8. Calculation 8.1 Calculate the net change and the percent change as follows: Symbol A a c D E 9 G H 1 J K L TABLE 4 Dimensions for Fig. 6 mm 4.76 6.35 7.14 13.49 38.10 44.45 52.38 63.50 76.20 88.90 127.00 in. 0.188 0.250 0.2B1 0.531 1.500 1.750 2.062 2.500 3.000 3.500 5.000 (Cn /T) x 100 where: CN = net change, A/p = final measurement, = initial measurement, CP = percent change, and T = film thickness. 9. Report 9.1 The report shall include the following: 9.1.1 Complete identification of specimens, including name and code number of coatings, size of the pipe, source, production date, production run number, and any other' information that may be pertinent to identification, 3 9.1.2 Film thickness of the specimen at the test location in millimetres (inches), 9.1.3 Temperature at which the test was conducted. D OKIU-THRU 1_ CT! rl 1 -tak- 4- RES'D- hftAT'L.-STL.. fj 1. M. 11 1L < f. il 9.14;, mchpsli ncKej 9.1.1 --! Hr -- F DRILL THRU 4.-PLACES ____LLJ z h)l-REa'P IViKr'L.-5TL FIG. 3 1050 Z-gEQ`D. MATlr&TL. DUP050298228 # G 17 !r Qo -e, ...I .. Ul o J.B'A- ~HOC.E-igRE.6iP. r------------------W ........ --.......~ -H irc JD1A. ID FIT MCROMETEK. |OE.ts>TH G.AsG.6. -1- ::' ;I ;: :i ^ r i-s ling rce,: ther tion 9.1.4 Final and initial measurements in millimetres nches), 9.1.5 Whether the weighted rod has caused penetration deformation, 9.1.6 Net penetration or deformation in: .millimetres jinches) and the percent penetration- or deformation, and 9.1.7 Number of hours or days to net penetration or deformation. 10. Precision 10.1 Precision Data are limited to two adjacent specimens taken from the same source coated pipe and assume that the coating process was uniform with respect to . pipe surface condition and coating material. Specimens that were not WT. 4.540 Kst fS.57 '.b.1 I mmm ill FIG. 5 1051 -D DIA,. O I- --Iil~ - ES OWPU.T TIP ) l-KEQ'D. MATl.- STAIN. STL. wr. .osoaKst (.ragjb.y DUP050298229  G 17 3- DtA. ^--9C?-- W HZBiya MATLr SPONGE RUBBER WELD HC-9 ( . WinsNUT (013) l-KCfl'D. SAME AS ore. EXCEPT AS SHOWN MAT'L.-STUi FIG. 6 adjacent in the as-produced condition or were taken from different lengths of pipe may represent' differing process conditions. 10.2 Repeatability--Initjal and final measurements should be 0,0127 mm (0.0005 in,) or 5 %. 10.3 Reproducibility--The results reported by one labora tory should not differ from those of another laboratory by more than 5 % of the net penetration. The American Society for Testing and Materials takes no position respecting the validity ofanypatent rights asserted In connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical ccmm/ttee and must be reviewed every five years and ifnot revised, either reapproved or withdrawn. Your comments are invited either forrevision.ofthisstandard orfor additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feef that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. use^ji tiotfc. *# 1052 DUP050298230 Designation: G 18 - 88 Standard Test Method for Joints, Fittings, and Patches in Coated Pipelines1 This standard is issued under the fixed designation G 18; tfie'number immediately following the designation indicates the year of original adoption or. in the case of revision, the year oflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () Indicates an editorial change since the last revision or reapproval. Scope 1.1 This test method describes determination of the comlarative corrosion preventative characteristics of materials gsed for applications to joints, couplings, irregular fittings, rid patched areas in coated pipelines. The test method is ipplicable to materials whose principal function is to. act as farriers between the pipe surface and surrounding soil enlironment. I? 1.2 The test method described employs measurements of 1'eakage`current, capacitance, and dissipation factor to indijgate changes in the insulating effectiveness of joint and patching materials. 1.3 This standard may involve hazardous operations and Equipment. This standard does not purport to address all of mhe safety problems associated with its use. ft is the responsi bility of the user of this standard to establish appropriate Safety and health practices and determine the applicability of Iregulatory limitations prior to use. 1.4 The values stated in SI units to three significant idecimals are to be regarded as the standard. jp. Referenced Documents 2.1 ASTM Standards: G12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel2 by f|3. Summary of Test Method 3.1 The test method consists of an immersion test where | coated pipe specimens, each containing a simulated joint, | tee, or patched area, are suspended in an electrolyte and placed under cathodic protection by connecting the speci mens to-the negative (--) terminal of a 6-V d-c power supply (see Fig. 1). An anode, also immersed in the electrolyte and connected to the positive (+) terminal of the power supply, completes the test circuit. Joint or patch performance is followed through periodic determinations of leakage current measured as voltage drops across a calibrated resistor in the i anode-to-cathode circuit. 3.2 Capacitance and dissipation factor measurements are used to supplement the periodic leakage current determina tions. 4. Significance and Use 4.1 The exposed metal surfaces at joints, fittings, and 1 This test method is under the jurisdiction of ASTM Committee G-3 on Durability of NonmetalHc Materials and is the direct responsibility of Subcom mittee G03.Q6 on Durability of Pipeline Coatings and Linings, Current edition approved Sept. 30, 1988. Published November 1988. Originally published as G 18 - 71 T. Last previous edition G 18 - 83. 2 Annual BookofASTMStandards, Vois 06.01 and 14.02. damaged areas in an otherwise coated pipeline will be subjected to corrosion if allowed to come in contact with the soil environment. The performance of joint and patching materials designed to function as protective coverings will depend upon such factors as the ability of the material to bond to both the pipe coating and exposed metal surfaces, the integrity of the moisture seal at lapped joints, and the water absorption characteristics of the joint material. 4.2 The existence of substantial leakage current through the coating joint, patch, or fitting is reliable evidence that the material has suffered a significant decrease in its perform ance as a protective barrier. In a similar manner, measured changes in joint capacitance and dissipation factor are useful because they are related to the water absorption rate of the joint material. Water permeating an insulating barrier in creases its capacitance and its progress can be measured through the use of a suitable impedance bridge. S. Apparatus 5.1 Test Vessel, nonconducting, shall be used to contain the test specimens. Dimensions of the vessel shall permit the followihg requirements: 5.1.1 The test vessel shall be large enough to allow for suspension of the specimens in a vertical position and equidistant from a centrally located anode. The specimens shall not touch either each other, the walls, or bottom of the test vessel. 5.1.2 The test vessel shall be deep enough to allow for immersion of the specimens in th'e electrolyte to the lower edge of the upper moisture shield (see Fig. 2). N' l--A commercially available, 42 L (11-gal) waste container of high-density polyethylene can be conveniently used as a test-vessel and will accommodate up to sue test specimens of a size indicated in 7.2. 5.2 Support Plate, fabricated from a nonconductive mate rial, to suspend the specimens in the test vessel. The support plate shall contain an access hole for the reference electrode. A typical test cell is illustrated in Fig. 3. 5.3 Anode, fabricated from 9.525 mm (0.375-in.) diam eter 300 series stainless steel rod, 609.6 mm (24.00 in.) long. Other inert anodes such as carbon or platinum may be used. 5.4 D-C Voltmeter, to serve the dual purpose of (/) mea suring leakage current as a potential drop across a 1,000-9 shunt in the measuring circuit and (2) measuring the potential of the test specimen with reference to a Cu-CuS04 half cell. The instrument characteristics for these functions shall be: 5.4.1 Voltage Range--50 pV full scale to 10 V full scale in overlapping 1 x and 3x ranges. 5.4.2 Accuracy--3 percent of full scale on all ranges. 5.4.3 Input Resistance--Greater than 10 M9 on all ranges. 1053 DUP0502 98231 G 18 METHOD A ME7H0P B LEAKAGE CLKRENT MEASUREMENTS LEAKAGE CURRENT, CAPACITANCE 5.10.2 Series Capacitance Range, 100 pF to 1100 accuracy 1 % 1 pF, whichever is larger. | 5.10.3 Dissipation Factor Range, 0.002 to i.O at 1 kHz accuracy 5 % or 0.001 dissipation, whichever is larger 5.11 Connectors--Miniature, pin-type, insulated jacks shall be used at the point of connection to each test specimen. The jacks serve two important functions: (/) they permit the disconnection of the specimen from the voltage source when the impedance bridge is in use, and (2) disconnection of the specimen from the test circuit also removes the effect of stray capacitance due to excessive lead length that may introduce error into impedance bridge measurements. 5.12 Foil Shield--As an additional safeguard against stray capacitance effects, wrap the entire test vessel in heavy-gage aluminum foil as shown in Fig. 3 and ground the shield. FIG. 1 Test Circuits 5.5 Thickness Gage--Measurements of coating thickness will be required for this test. Any instrument suitable for use with Test Method G 122 can be used. However, the choice of measuring gage shall be compatible with the joint coating thickness that will be encountered in the test. 5.6 Ohmmeter--Measurements for end-cap integrity shall be made with a suitable ohmmeter capable of reading resistance to an upper,limit of 1000 MQ .5 %. 5.7 Reference Electrode--A Cu-CuS04 half cell of con ventional glass or plastic tube with porous plug construction, but preferably not over 19.05 mm (% in.) in diameter, having a potential of --0.316 V with respect to the standard hydrogen electrode. N' 2--A saturated calomel half cell may be used, but measure ments made with it shall be converted to the Cu-CiiSO, reference for reporting by adding -Q.072 V to the observed reading. : 5.8 Voltage Source--A battery or rectifier-type power supply shall be used to maintain a potential difference of 6.0 0.1 V dc between each of the test specimens and the Cu-CuS04 half cell. Where multiple specimens are tested, a suitable voltage-dividing circuit will be required for indi vidual control of the voltage applied to each specimen. 5.9 Circuit Wiring from the anode to specimen shall be of No. 18 Awg insulated copper. A switch for disconnecting each specimen from its voltage source shall be included in the circuit. A 1000 1 percent, 1-W (minimum) precision resistor shall be placed in the anode-to-cathodc circuit as a shunt for current. A diagram illustrating the test cell wiring appears as Fig. 1. 5.10 Capacitance Bridge--Measurements of specimen ca pacitance and dissipation factor shall be made with a low-voltage a-c, resistive ratio arm-type bridge3 having the following characteristics: 5.10.1 Oscillator Frequency, 1 kHz 2 % tolerance. 3 Instruments found to meet these requirements arc the General Radio Type 1650-B Impedance Bridge and the Heath Co, Model IB-28 Impedance Bridge (Kit). 6. Materials 6.1 Electrolyte--The electrolyte shall consist of potable tap water with the^ddition of 3 weight percent of technicalgrade sodium chloride. 6.2 Materials for sealing the ends of the specimens may consist of waxes, epoxies,,or other suitable materials. How ever, they should have a dielectric constant in the range from 2 to 6, and exhibit a low water-absorption rate. It is also important that the end-cap material maintains good adhe sion to any coated pipe surfaces throughout the test period. 7. Test Specimen 7.1 The joint specimen shall be prepared from a represen tative piece of 60.325 mm (2.375 in.) outside diameter, Schedule 40, production-coated pipe. 7.2 Each piece of coated pipe shall be 381 mm (15.0 in.) long and serve as a carrier for the particular joint material to be tested. 7.3 The simulated coatingjoint shall be made by cleaning away a 101.6 mm (4.0-in.) band of pipe coating starting from a point 203.2 mm (8.0 in.) below the upper end of the pipe. The coating may be removed by power brushing or any other suitable device that will remove all of the coating in the area indicated and leave a dean metal surface behind. 7.4 The lower end of the test specimen shall be plugged flush with a stopper and sealed or capped with a material meeting the requirements of 6.2. 7.5 When used, the primer shall be applied to the test specimen in sufficient quantity to coat the test specimen from a point 88.9 mm (3.50 in.) below its upper end and ending at a point 317.5 mm (12.5 in.) from the upper end. This will allow for a 12.7-mm (0.5-in.) band of excess primer beyond each tape margin. 7.6 The joint material to be tested shall be applied to the prepared pipe specimen (using a spiral wrap for tapes) and starting from a point 101.6 mm (4.0 in.) below the upper end of the pipe section and ending at a point 304.8 mm (12.0 in.) from the upper end. The 203.2 mm (8.0 in.) ofjoint material thus applied should overlap the bared section of pipe by 50.8 mm (2.0 in.) at each end. This distance represents the typical cut-back distance encountered in the field joining, through welding, of coated pipe in 60.325 mm (2.375 in.) outside diameter size. A diagram of the joint specimen appears as Fig. 2. 1054 he s ne i 1 'ce< G ol 7.8i d:s{, dce| : th< .12: Ti 8J.( 70 ta tl 9-V Indmyf(t ,d;4 |0.lf ioi bseij esse) nidvf. aatel' | spepi| ,...4 f i W, Not. D UP 0502 98232 fl G 18 >F 1 7.7 The manner of applying the joint material shall be |one in accordance with the manufacturer's specifications. he supplier of the joint material should specify the desired |ine interval between the application ofthe material and the art of the test. N' 3--Materials that are intended for use as a field-applied patch iyer damaged areas on coated pipelines can be tested using the same procedures, with the patching compound applied, instead, to the bared ftea of the simulated joint. 7.8 The upper 76.2 mm (3.0 in.) of the completed joint lest specimen shall be coated with the material used for the power end cap. This moisture shield can be conveniently hade, in the case of some waxes and epoxies, with several |uccessive brush or dip-applied applications. The thickness ijf the moisture shield should be approximately 3.175 mm |p. 125 in.). . Testing Temperature 8.1 Perform all tests at a room temperature of 21 to 25"C 70 to 77*F). . Preliminary Test Measurements 9.1 Coating and Joint Thickness--Measure and record he thickness of the base coating which lies exposed at each end of the test joint. Measurements shall be made in Accordance with Method G 12. In a like manner, measure and record the average thickness of the joint covering. 110. Procedure for Leakage Current Measurements 10.1 Suspend the joint test specimens in the test vessel, ^observing the clearances specified in 5.1.1 and 5.1.2. Fill the jjvessel with electrolyte, bringing the fluid level up to a point tmidway between the end cap and the lower edge of the joint Itnaterial. 10.2 Connect one terminal of the ohmmeter to the test I'specimen and the other terminal to the central anode. The N' --Alt dimensions are in millimetres with inches in parentheses. FIG. 2 Joint Test Specimen anode should be in contact with the electrolyte. Measure the apparent sample-to-anode resistance in ohms. The reading shall remain above 1000 MQ for 15 min. Readings below this value probably indicates a faulty end-cap seal which should be repaired before the joint specimen is totally immersed. 10.3 Totally immerse the joint test specimens up to the lower edge of the moisture shield. This level shall be maintained throughout the test period by regular additions of tap water. The test shall be performed at room tempera ture. 10.4 Connect each joint test specimen in series with a 1000-0 1 % (1-Wj resistor, a suitable switch, and the negative (--) terminal of the voltage source. 10.5 Connect the central stainless steel anode to the positive (+) terminal of the voltage source. 10.6 Energize the voltage source. Adjust the voltage to each specimen by connecting a voltmeter between each sample and the Cu-CuS04 half cell and varying the- voltage output until 6,0 V are measured between sample and half cell (see Fig. 1). 10.7 As soon as the circuit is energized and voltage adjusted to each joint test specimen, measure and record the voltage across each 1000-fi shunt resistor. 10.8 Measure and record the closed circuit potential, EB, and open circuit potential, E0, of each joint specimen with reference to the saturated Cu-CuS04 half cell. N' 4--Any drop in closed circn t potential (B) of a joint specimen greater than 20 % of the terminal voltage (,) probably indicates a developing current leak in the joint area. In a like manner, any open circuit potential (EJ greater than 0.05 V may indicate the presence of a developing conductive path across the test joint. (Both voltages are referenced to the Cu-CuS04 half cell.) 10.9 Using the d-c voltmeter in 5.4 measure and record the voltage appearing across the terminals of the voltage supply. 10.10 Continue, on a periodic basis, the measurements specified in 10.7 through 10.9. Calculate the apparent joint 1055 DUP050298233 G 18 resistance by the method described in 12,1. 10.11 Prior to removal, reexamine a suspected joint failure to confirm that any observed drop in joint resistance is not due to a faulty end-cap seal. This can best be accomplished by removing the specimen from the test cell and allowing it to dry. When dry, reimmerse it to just above the level of the: lower end cap and check the integrity of the cap by the method outlined in Section 8. 11. Procedure for Measurement of Capacitance and Dissipa tion Factor 11.1 The series capacitance and dissipation factor be tween each joint sample and the central stainless-steel anode shall also be measured. These measurements shall be made at the time of initial immersion and continued on an identical schedule with the voltage readings. They shall be made in the following manner: 11.2 Temporarily disconnect the test specimen from the voltage source. Connect the impedance bridge between the test specimen and stainless-steel anode. Energize the bridge and measure the equivalent series capacitance, C, and dissipation factor, DF, or the test specimen using a "null" technique to balance the measuring bridge. 11.3 A continued rise in joint capacitance and dissipation factor from the values recorded at the time of initial immersion, will indicate progressive absorption of water by the joint material. 11.4 The joint test shall continue for 180 days or until the joint resistance falls to a value of4600 Q for 1 m2 (50 000 Q for 1 ft2) of immersed joint surface. 12. Calculations 12.1 Joint Resistance--Calculate the resistance, Rjt for the joint sample as follows: Rj = 1000 Al(ED - Ej/AJ where - resistance, fl/cm2 (D/ft2), A immersed sample area (excluding end cap), cm2 (ft2), Eb closed circuit potential of sample (reference Cu- CuS04), V (switch closed), Ea open circuit potential of sample (reference Cu- CuS04), V (switch open), and EF voltage across I000-R shunt resistor, V, (switch closed). 13. Report 13.1 All test reports shall include the following: 13.1.1 Complete identification of the joint specimen in cluding: 13.1.1.1 Name and code number of the base coating. 13.1.1.2 Thickness of the base coating, 13.1.1.3 Name and code number of the joint material including type (that is tape, two-part mix, etc.), 13.1.1.4 Method of application of joint material, in cluding amount of overlap. 13.1.1.5 Where applicable, the width and thickness of the joint material (tapes), 13.1.1.6 Where applicable, the name, code number, and type of primer, 13.1.1.7 Where applicable, the method of application of primer,, 13.1.1.8 Average thickness of the joint material, as ap plied, and . 'i 13.1.1.9 Dates of starting and terminating the test and other information that may be pertinent. 13.2 The following readings shall be recorded on a peri odic basis: 13.2.1 Voltage across the 1000-0 shunt resistor, E%, 13.2.2 Closed-circuit potential of the joint specimen refer enced'to the Cu-CuS04 half cell, EB, 13.2.3 Open-circuit potential of the joint specimen refer enced to the Cu-CuS04 half cell, Ea, 13.2.4 Terminal voltage at the power supply, and 13.2.5 Calculated value ofjoint resistance, 13.2.6 Initial series capacitance of the joint sample, and ` 13.2.7 Initial dissipation factor of the joint sample. N' 5--The frequency of experimental readings will depend upon the performance of each joint specimen. Specimens that show a high rate ofchange may require more frequent watching if the point of failure is to be recorded. Normally, weekly readings have been found to be adequate. Joint performance can be conveniently followed.through plots of Joint Resistance versus Time and Dissipation Factor versus Time in semilogarithmic coordinates, and Capacitance Change versus Time in rectangular coordinates. 14. Precision 14.1 Due to the range of joint coating formulations, thicknesses, densities, etc. found among commercially avail able materials, the over-all accuracy and reproducibility of test results by these methods will tend to be poorer than those expected on straight runs of coated pipe. The fact that most joint materials are hand-applied introduces an inherent factor of variability into the test results. The basic purpose of these methods is to provide a means for the comparative screening of combinations of joint materials and base coatings for insulating effectiveness. 14.2 The precision (reproducibility) of the joint resistance determination by these methods is considered to be such that when two tests are performed consecutively on the same specimen and under identical conditions of application, the difference between the two results may normally be expected not to exceed 10 % of their mean. The American Society for Testing and Materials takesno position respecting the validity of any patent rights asserted in connection with any itam mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed td ASTM Headquarters. Your comments will receive careful consideration af a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1915 Race St., Philadelphia, PA 19103. 510 , Sco] ,1.1 : dative eel P ial. I type hermc f 1.2.': lifferer [fer^i. iton^ 1.4-r (md eql. all of tesponi, approve applied " 1-5 ! decima . i Reft-' Z.i ; Gil -Ff G (.3, Slui 3.1 litectiVet pan el'ef. Jareas | conneif coatinjp isons E* Si| 4. 4.1 i danaa^.; contrii; 1056 DUP050298234 Designation: G 19 - 88 materia], srial, in:ss of the ber, and ation of Standard Test Method for Disbonding Characteristics of Pipeline Coatings by Direct Soil Burial1 This standard is issued under the fixed designation G 19; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. , as ap- est and a peri- s> n refer- a refer- , and id upon a high f failure i to be ;h plots Time in 'ime in Scope 11.1 This test method describes the determination of the llative disbonding characteristics of damaged coatings on feel pipe by cathodic protection potentials in direct soil [trial. This test method is intended to apply to the testing of i types of nonmetallic pipeline coatings and tapes including iermoplastics, thermoset, and bituminous materials. 1.2 Results may vary widely when test sites are in Ferent geographical areas of the country, and even in Different localities. 1.3 This test method is limited to nonconducting, or |onmetallic pipe coatings and is not applicable to con|ucting materials such as zinc coatings on steel pipe. 1.4 This test method may involve hazardous operations and equipment. This test method does not purport to address |ll of the safety problems associated with its use. It is the tfsponsibility of the user of this lest method to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1.5 The values stated in SI units to three significant Decimals are to be regarded as the standard. tions, availity of than t that erent e of alive base ance that iame , the cted . Referenced Documents 2.1 ASTM Standards: G12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel2 G62 Test Methods for Holiday Detection in Pipeline Coatings3 |3. Summary of Test Method 3.1 Apparatus and materials are described whereby proitective coatings on steel pipe are subjected to disbonding by Ian electrical stress. Specimens with intentionally damaged lareas are buried in soil at an outdoor site and electrically jconnected to a magnesium anode. After test, the disbonded fcoating is removed, the exposed area measured, and comparfisons are made to other specimens similarly exposed. j 4. Significance and Use 4.1 Coated pipe is seldom, if ever, buried without some 1 damage to the coating. Hence, an actual soil-burial test can | contribute significant data, provided the method of testing is 1 This test method is under the jurisdiction of ASTM Committee G-3 on p Durability of Nometallic Materials and is the direct responsibility of Subcom mittee (303.06 on Durability of Pipeline Coatings and linings. Current edition approved May 27, 1988. Published July 1988. Originally published as G 19 -71 T. Last previous edition G 19 - 83. 2 Annual Book ofASTM Standards, Vols 06.01 and 14.02, 3 Annual Book ofASTM Standards, Vol 14.02. controlled and the test specimen monitored and the relation ship between the area disbonded, the currefft demand, and the mode of failure is fully understood. 4.2 Means are provided for measuring and following the electrical potential and current flow and relating these data to the final measurement of disbonded area. 5. Apparatus- 5.1 Anode--A standard packaged magnesium anode, minimum 4.082 kg (9 lb), with a factory-sealed, 4107-cmil (14-gage Awg) minimum, insulated copper wire shall be used. A solution potential of not less than -1.45 V with respect to a copper-copper sulfate reference electrode is required. Use sufficient anodes to maintain required poten tial. 5.2 Connectors--The wiring circuit from anode to test specimen and from specimen to reference electrode should be 4107-cmil (14-gage Awg) minimum insulated copper wire. Attach the wires to the test specimen as shown in Fig. 1 by soldering or brazing at the air-exposed end, and coat the place of attachment with insulating material. A junction box is optional for connecting the resistor in series between the anode and the test specimen. 5.3 The instruments used shall include the following: 5.3.1 Voltmeter, a suitable instrument, such as a high impedance (>10mft) analog multimeter having a sensitivity of 50 000 fi/V minimum and a multiple range from 0.01 to 2 V for direct current is used for measuring the potential between specimen and the reference electrode,'' current between specimen attd~anode, and the resistance of the circuit. The same instrument shall be used for measuring current between specimen and anode. Alligator clips on the leads are permissible. 5.3.2 Volt-Ohm-Meter for measuring resistance of the circuit. 5.3.3 Reference Electrode, consisting of a copper-copper sulfate half cell in a conventional glass or plastic tube with porous plug construction, but preferably not over 19.05 ram (% in.) in diameter, having a potential of -0.316 V with respect to a standard hydrogen electrode. A calomel elec trode may be used, but measurements made with it should be converted to the copper-copper sulfate reference electrode for reporting, by adding -0.092 V to the observed reading. 4 A pipe-lo-soil Voltmeter-Ammeter, Agra Engineering Co., Tulsa, Okia., has been found suitable for this test. 1057 DUP050298235 G 19 5.3.4 A suitable instrument is used to measure the soil resistivity using the four-pin method.5 Pins should be spaced 762 mm (30 in.) apart. 5.3.5 Thickness Gages, to be used in accordance with Test Method G 12. 5.3.6 Holiday Tools--Holidays in the specimen are made with conventional drills of the required diameter. A 9.525nim (0.375-in.) drill modified by substantially reducing the cone angle has been found effective in preventing perforation of thin-wal! pipe or tubing. A sharp-pointed knife with a safe 5 A Vibroground instrument, Associated Research Inc., 3758 Belmont Ave., Chicago, IH., has been found suitable for measuring soil resistivity. handle is required for removing disbonded coalings to make physical examinations. A micrometer-type depth gage is usedfor measuring coating thicknesses at the edge of holidays. 5.3.7 Holiday Detectors--Selected i'11 accordance with. Test Method G 62. 6. Test Specimen 6.1 A 1219.2 mm (48-in.) long specimen shall be prepared with its surface preparation and coating procedures equiva lent to that of production coated' pipe- Only holiday-free specimens may be used in this test and four samples should be prepared. 1058 DUP0502 98236 G 19 <MBS.2 Measure the coating thickness of all specimens at four Hfiints 90 deg apart and approximately 355.6 mm (14 in.) jBfcm each end. SHj6.3 Cap and seal one end of each specimen. Check the seal tjlifiYi current leakage before and after test by immersion in 1 {Weight percent sodium chloride solution for Vz h. Test with JHK ohmmeter sensitive to at least 1 Mft. M6.4 Provide the unsealed end of the pipe with two lengths JB( insulated 4107-cmil (14-gage Awg) copper wire as in 5.2. '3( 6.5 Make 3 holidays 304.8 mm (12 in.), 457.2 mm (18 jH|,), and 609.6 mm (24 in.), respectively, from the sealed end R the pipe by drilling holes through the coating so that the ; Iffiill will fully enter the steel. The center holiday is to face the jHlode with the remaining two holidays facing 180 deg away ' ! jgpnn the anode. The drill diameter may not be less than two ! '' 'Irfimes the coating thickness, and never smaller than 9.525 Am (0.375 in.) in diameter. Do not perforate the steel wall of ' ' K PiPe- With thin-wall steel pipe where there is danger of fijrforating the pipe, start the holiday with a standard 60-deg jpme-point drill and finish with a substantially reduced q^ne-angle drill. ` ' oS 116-6 To prevent mechanical damage, apply a spiral wrap of Kaitable tape from approximately 152.4 mm (6 in.) from the Slip of the pipe specimen to 457,2 mm (18 in.) from the top. ; illyhen the test specimens are buried, the taped area will i iBtend 152.4 mm above and 152.4 mm below ground. ' 3? 6.7 The specimen test area will consist ofthe area between lime edge of the bottom end seal and the ground level. The JBottom end-seal area is not considered part of the area tested. TPiny suitable diameter and length of pipe may be used, but She buried area should not be less than 23 227.2 mm2 (36 4Eln.2). An area of 93 000 mm2 (1 ft2) has been found " 'ij preferable. JP. Test Site Iff 7.1 Any level location may be used, provided the site will iKiot be disturbed for the duration of the test. ' ke na usea- jH$. Procedure jj|; 8.1 Lay out the test site with stakes so that the anode ^location will be the center of a circle as shown in Fig, 1. Xtocaje the pipe specimens 20 apart around the circumfer. 3 ence so that the surface of the anode when placed in the "Kcenter will be 609.6 mm (24 in.) from the nearest holiday of fcCach specimen equally. Three specimens can thus be pro spected by one anode, W ^ Installation of Test Specimens: m 8.2.1 Dig suitable holes with an auger or posthole digger t0 accomrn0(jate the anode and test specimens at the test iared riva-free .ould $, 8.2.2 Insert the anode at the center of the circle. The center of the anode should be 457.2 mm (18 in.) below mground. Pipe specimens should be inserted so that 304.8 mm fi(12 in.) are above the ground level, and oriented so that the E single intentional holiday faces the anode and the remaining two holidays are 180 deg away from the anode. Maintain a 1L distance of 609.6 mm (24 in.) between the surface of the a anode and the nearest specimen and holiday. a' 8.2.3 Refill all holes with soil or a soil and water slurry. I]1 Firmly tamp the soil so that it is in intimate contact with the specimen and anode. No wood or other foreign material should contact the pipe coating or the anode. 8.3 Electrical Measurements: 8.3.1 Determine in several areas the Soil resistance in ohm-centimetres by the four-pin method. 8.3.2 Measure the initial pipe to soil potential with reference to a copper-copper sulfate half cell with the electrode 609.6 mm (24 in.) from the pipe as shown in Fig. 1. Record the closed-circuit potentials. 8.3.3 Connect the anode lead to one test specimen lead at the junction box with a 10 Q 1 % wire-wound resistor connected in series between the anode and test specimen. 8.3.4 Measure the voltage..E, across the 10-Q resistor, R, and convert to current, I as follows: I = E/R -- EjXQ 8.3.5 Measure the polarized potential, in volts with the analog multimeter described in 5.3.8 connected between the test specimen and the reference electrode as follows: 8.3.5.1 Disconnect the anode from the test specimen while closely observing the analog multimeter. As the instrument pointer falls, it will dwell significantly at the polarized value before receding further. The dwell point is the polarized potential. 8.3.6 Determine electrical measurements at 30-day inter vals for a test period of 18 months or longer depending on soil conditions. 9. Report 9.1 The report shall include the following: 9.1.1 Complete identification of the test specimens, in- eluding name and code number of coating, size of the pipe, source, production date, production run number, and any other information that may be pertinent to identification. 9.1.2 Date of starting and of terminating the test-. 9.1.3 Coating thickness of the test specimen before testing. 9.1.4 After subtracting the initial holiday areas, report the total disbonded area, average disbonded area, and disbonded area at each holiday in square millimetres (square inches) after testing. 9.1.5 Condition of the pipe surface under the_disbonded coating. ___ 9.1.6 Pipe-to-soil potentials, initial readings and at 30-day intervals. 9.1.7 Current readings between anode and pipe speci mens, initial readings and 30-day intervals. 9.1.8 Soil resistivity readings in ohm-centimetres. 9.1.9 Polarized potentials, initial readings and 30-day intervals. 10. Precision 10.1 Precision data are limited to two adjacent specimens taken from the same production-coated pipe, assuming that the production process was uniform with respect to pipe surface condition and coating material. Specimens that were not adjacent in the as-produced condition, or were taken from different lengths of pipe may represent differing process conditions. 1059 j j ; ij "\ l j f 1 j j j Tl mugffW DU P0502 98237 # G 19 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard; Users of this standard are expressly advised that determination of the validity of any such patent rights, end the risk of Infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any (/me by the responsible technical commftfee and must be reviewed every five years and Ifnot revised, either reapproved or withdrawn. Yourcomments are Invitedeither forrevision of this standard or foradditional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical corom/ftee, which you may attend. If you fee) that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 7916 Pace St., Philadelphia, PA 19103. to 1060 gyironj In of* jportefl gflect q tei- ]W equ\ | */# fpwprj^. pplicdfo . 'Rcfe: h.i Ai ID 543 , Reaf 1ID.883 f.G8 Coa|:G12 Fils 1 G-rfi C<f>a Suiju ft '|s3ii jr;v doSeC ; Jmg-tejiri i |e' test | lispeete :fcsts lethod Test Me'; specimen"' ending |*> i. Signife 4.i 't |: 'This t|i . Durability^ mittce G03| Current Jj ^published t 1 Annmfk lAnmiae> DU P05 02 982 38 Designation: G 20 - 88 Standard Test Method for Chemical Resistance of Pipeline Coatings1 This standard is issued under the fixed designation G 20; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year oflast reapproval. A superscript epsilon (c) indicates an editorial change since the last revision or reapproval. Scope ,j 1.1 This test method is intended for evaluating the resistmce of pipe coating materials when exposed to various concentrations of reagents or suspected soil contaminants, "fie test serves as a guide to investigators wishing to compare jite relative merits of pipe-coating materials in specific 1Environments. The choice of reagents, concentrations, dura ii tion of immersion, temperature of test, imported are necessarily arbitrary and and properties to should be chosen be to reflect conditions known to exist along the pipeline right- M-way. 1.2 This test method may involve hazardous operations mnd equipment. This test method does not purport to address ?/ of the safety problems associated with its use. It is the :sponsibility of the user of this test method to establish Appropriate safety and health practices and determine the Applicability ofregulatory limitations prior to use. . Referenced Documents 2.1 ASTM Standards: ,D 543 Test Method for Resistance of Plastics to Chemical Reagents21 ,' j( D883 Definitions of Terms Relating to Plastics2 G 8 Test Methods for Cathodic Disbonding of Pipeline Coatings3 G 12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel3 G 17 Test Method for Penetration Resistance of Pipeline Coatings (Blunt Rod)3 3. Summary of Test Method 3.1 This test method consists of an immersion-type test in closed container where coated pipe specimens are in long-term contact with both the liquid and vapor phase of ||he test reagent. Specimens exposed in this manner are Inspected for visible signs of chemical attack. Subsequent Jtests for cathodic disbonding in accordance with Test iMethod G 8, or penetration under load in accordance with (Test Method G 17, may be applied to determine if the ^specimens have undergone any loss of mechanical or [(bonding properties. 4. Significance and Use 4.1 The data obtained for short-term tests are of interest 1 This test method is under the jurisdiction of ASTM Committee G-3 on | Durability of Nonmetallic Materials and is the direct responsibility of Subcomf mittee G03.06 on Durability of Pipeline Coatings and Linings. Current edition approved May 27, 1988. Published July 1988. Originally published as G 20 - 71 T. Last previous edition G 20 - 83. 2 Annual Book ofASTM Standards, Vol 08.01. 3 Annual Book ofASTM Standards, Vols 06.01 and 14.02. only in eliminating the most unsuitable materials or for indicating a probable order of resistance in any particular media. 4.2 Test conditions should take into account the manner and duration of immersion, the reagent, the . temperature of the system, the area exposed above and below the liquid level, and other performance factors selected for the partic ular test. 5. Apparatus 5.1 Thickness Gage, capable of measuring the coating thickness in the manner prescribed by Test Method G 12. 5.2. Test Container--A transparent closed container, sized to completely encase the pipe specimen and large enough to provide adequate exposure to both the liquid and vapor states of reagent. N' 1--For example, a 2-L (2.0-qt) capacity. Mason-typejar with a 70-mm (2.75-in.) diameter neck has been found suitable for use with 2 in. pipe and is illustrated in Fig. 1. 5.2.1 To avoid pressure build-up within the test con tainers, the threaded cup shall be replaced with a solidrubber stopper. A positive venting device, such as a water seal, shall be used when testing with volatile solvents at elevated temperatures. 5.2.2 A separate container shall be used for each test specimen. 5.3 Oven or Constant-Temperature Room or Bath--To ensure uniformity of test results, the test cells and specimen shall be maintained at the test temperature 5C (9F) over the duration of the test period. 5.4 Auxiliary Testing Devices--Supplemental equipment used to determine specific mechanical properties of speci mens before and after immersion shall conform-to the requirements prescribed, in the .applicable ASTM test method. 6. Test Specimen 6.1 The test specimen shall be prepared with its surface preparation and coating procedures equivalent to that of coated pipe. A control specimen shah be retained for comparison. 6.2 In order to utilize the test container specified in 4.2, the pipe specimen, with end caps, shall be restricted to a maximum overall length of 180 mm (7.0 in.) and a diameter of 65 mm (2.5 in.). 6.3 Both ends of the pipe specimens shall be plugged with inert stoppers and coated with an epoxy-base coating mate rial. 6.4 Specimens with Holidays: 6.4.1 A holiday shall be made in the surface of the coated pipe specimen at a point 25 % of the distance between the 1061 DUP050298239 # G 20 end caps. It shall be made by drilling a radial hole through the coating so that the angular cone point of the drill will fully enter the steel where the cylindrical portion of the drill meets the steel surface. The drill diameter shall not be less than three times the coating thickness, but it shall never be smaller than 6 mm (0.25 in.) in diameter. The steel wall of the pipe shall not be perforated. 6.4.2 A second identical holiday shall be drilled into the coating surface at a point 25 % of the distance between the end caps of the specimen (see Fig. 1). Both holidays should lie in the same pipe axis. 6.5 Specimens without intentional holidays shall also be prepared for testing. N' 2--Intentions] holidays shall be made in only those specimens for which a; comparison of disbonding properties is desired. Other samples used for supplemental mechanical testing shall be run without holidays. 7. Reagents 7.1 The reagents selected for coating-resistance tests should be those anticipated to occur in the environment or in the product being carried in the pipeline at the tempera tures and in the concentrations expected. The numbers in parentheses refer to the list of standard reagents given in Section 4 of Test Method D 543. 7.1.1 Acetic Acid (5 %) (4.4.2). 7.1.2 Acetone (4.4.3). 7.1.3 Carbon Disulfide. 7.1.4 Gasoline. 7.1.5 Hydrochloric Acid (10 %) (4.4.23). 7.1.6 Kerosine (4.4.28). 7.1.7 Lime Water, Saturated. 7.1.8 Methyl Alcohol (4.4.29). IAS Methyl Ethyl Ketone. 7.1.10 Nitric Acid %) (4.4.33). 7.1.11 Sodium Carbonate Solution (20 %) (4.4.38). 7.1.12 Sodium Chloride Solution (10 %) (4.4.40). 7.1.13 Sodium Hydroxide Solution (10 %) (4.4.42). 0GI.ASS U WITH 7.1.14 Sulfuric Acid {30 %) (4.4.46). 7.1.15 Toluene (4.4.48). 7.1.16 Transformer Oil (4.4.49). 7.1.17 Trichlarethylene. 7.1.18 Other selected environments. 8. Precautions 8.1 Safety precautions should be taken to avoid personal contact, to eliminate toxic vapors, and to guard against explosion hazards in accordance with the hazardous natUK of the particular reagents being used. 9. Procedure 9. t Place a single specimen in a vertical position in each test container. 9.2 Fill the container with the selected reagent so that the liquid level covers one half of the coated pipe specimen up to a point midway between the two intentional holidays. Stopper the 704 Container to prevent evaporation of thereagent and against,contamination. 9.3 Maintain the reagent level at the original level. 9.4 The basic immersion test for a particular coating material shall consist of twelve specimens, six with holidays and six without, each in an individual test cell. Remove duplicate samples of each from the test at 30,60, and 90 day ` intervals. Additional investigations of pre- and post immer sion mechanical properties will require additional specimens. It is recommended that in all cases provisions be made for duplicate test specimens. 9.5 Remove the specimen after 30, 60, and 90 days of immersion. Wash with running water all specimens removed from acid, alkali, or other aqueous solutions and wipe them dry with a soft, clean, cotton cloth or paper tissue. Specimens removed from volatile solvents such as acetone, alcohol, etc., need no rinsing before wiping dry. 9.6 Observe and report before, immediately after, and 2 h later the appearance of specimen after exposure to reagent on the basis of visual examination for evidence of loss of gloss, developed texture, decomposition, discoloration, softening, swelling, injury, bubbling, blistering, cracking, solubility, etc. as defined in D 883. 9.7 Mechanically probe each of the intentional holidays in accordance with Section 8.3.3-of Test- Method G 8 to see if there has been any loss of coating bond during the test period. 9.8 Perform other planned mechanical tests to determine ifany degradation of coating properties has occurred through reagent exposure. A--70 mm (2.75 in.) Jar Opening S--45 mm (1.75 in.) Holiday Location C--90 mm (7.00 in.) Length of Pipe Specimen N' --Dimensions shown for 2 in. IPS pipe. FIG. 1 Chemical Immersion Test Schematic of Test Ceil 10. Report 10.1 The report shall include the following: 10.1.1 Complete identification of the material tested, including type, source, manufacturer's code, and previous history, 10.1.2 Method of preparing test specimen, 10-1.3 Temperature of test, 10.1.4 Description of media, including ASTM designa tion, 10.1.5 Duration of immersion, 10.1.6 Outside diameter of test specimen, 10.1.7 Initial thickness of coating. 1062 11 ij /I. DUP050298240 # G 20 'ersim.il i nature 0.1.8 General appearance of specimen after immersion, D.1.9 Immersion area in square millimetres (square |es), .1.10 Vapor phase area in square millimetres (square fees), and |p. 1.11 Disbonded area after immersion in square jimetres (square inches). 11. Precision and Bias 11.1 As there are no direct measurements involved with this test method, no precision and bias statement is neces sary. Measurements made by procedures for other test methods should refer to the precision and bias statements therein. Tb& American Society tor Testing and Materials takes no positbn respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are express// advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. ii each hat the', tup to' lidays; df the^I This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either torrevision ofthis standard or tor additional standards.: and should be addressed to ASTM Headquarters, your comments wilt receive careful consideration at a meeting of the responsible technical committee, which you may aitena. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. dating;;1 'lidayji :taove`' 0 day*' rimermens.* Je (dip ,ys of ! tb\cd them l mens , etK,; i2h it on (toss, ling, , etc., ys in ee if test line 1 ugh |r v ; :ed, ous 1063 DU P0502 98241 Designation: G 23 - 90 Standard Practice for Operating Light-Exposure Apparatus (Carbon-Arc Type) With and Without Water for Exposure of Nonmetailic Materials1 This standard is issued under the fixed designation G 23; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year ofiast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon U) indicates an editorial change since the last revision or reapprovaL This standard has been approved fot use by agencies of the Department of Defense. Consul! the DoD Index ofSpecifications and Standardsfor the specific year of issue which has been adopted by the Department ofDefense. 1. Scope 1.1 This practice covers the basic principles and operating procedures for light-exposure apparatus with and without water spray employing a carbon-arc light source. 1.2 This practice does not specify the exposure conditions best suited for the material to be tested. It is limited to the method of obtaining, measuring, and controlling the condi tions and procedures of the exposure. Sample preparation, test conditions, and evaluation of results are covered in ASTM test methods or specifications for specific materials. N' 1--Attention is called to the following test methods and practices for more information on use of this practice for specific materials; Practices D 529, D 822, D 904, D 1499, D 3361, D 3815, E 765 and Test Methods C 732, C 734, C 74], D 750, D 3424 and D 3583, 1.3 This practice includes four procedures: 1.3.1 Method 1--Continuous exposure to' light and inter mittent exposure to water spray, 1.3.2 Method 2--Alternate exposure to light and darkness and intermittent exposure to water spray. 1.3.3 Method 3--Continuous exposure to light without water spray. Specific exposure conditions for testing fabric are found in AATCC Test Method 16A. 1.3.4 Method 4--Alternate exposure to light and darkness without water spray. 1.4 The values stated in SI units are to be regarded as the standard. The inch-pound unit equivalents of the SI units may be approximate. . 1.5 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: C 732 Test Method for Aging Effects of Artificial Weath ering on Latex Sealants3 C 734 Test Method for Low-Temperature Flexibility of Latex Sealants After Artificial Weathering2 C 741 Test Method for Accelerated Aging of Wood Sash Face Glazing Compound2 D 529 Practice fdr Accelerated Weathering Test of Bitu minous Materials3 (Carbon-Arc Method) D 750 Test Method for Rubber Deterioration in CarbonArc or Weathering Apparatus4 D 822 Practice for Conducting Tests on Paint and Related Coatings and Materials Using Filtered Open-Flame Carbon-Arc Light- and Water-Exposure Apparatus5 D904 Practice for Exposure of Adhesive Specimens to Artificial (Carbon-Arc Type) and Natural Light6 D1499 Practice for Operating Light- and Water-Exposure Apparatus (Carbon-Arc Type) for Exposure of Plastics7 D3361 Practice for Operating Light- and Water-Exposure Apparatus (Unfiltered Open-Flame Carbon-Arc Type) for Testing Paint, Varnish, Lacquer, and Related Prod ucts Using the Dew Cycle5 D 3424 Method for Evaluating the Lightfastness ofPrinted Matter5 D 3583 Methods of Testing Joint Sealant, Hot-Applied, Elastomeric Type for Portland Cement Concrete Pave ments, or Joint Sealant, Hot-Applied Elastomeric, JetFuel-Resistant Type, for Portland Cement Concrete Pavements8 D3815 Practice for Accelerated Aging of Pressure Sensi tive Tapes by Carbon-Arc Exposure Apparatus9 E 765 Practice for Evaluation of Cover Materials for Flat Plate Solar Collectors10 2.2 AATCC Standards:" Blue Wool Lightfastness Test method 16A Colorfastness to Light, Carbon-Arc Lamp, Continuous Light 1 This practice is under the jurisdiction ofASTM Committee G-3 on Durability of Nonmetailic Materials and is the direct responsibility of Subcommittee G03.03 on Simulated and Controlled Environmental Tests. Current edition approved Oct. 26, 1990. Published December 1990. Originally published as E 42 - 42 T. Last previous edition G 23 - 89. Replaces E 42 - 69 and combines G 23 - 69 (1975) and G 25 - 81, Practice G 25, Standard Recommended Practice for Operating Enclosed Carbon Arc Type Apparatus for Light Exposure of Nonmetailic Materials, is to be discontinued since it now is covered in this edition of C 23 and its Methods 3 and 4. 2 Annual Book ofASTM Standards, Vol 04.07. 3 Annual Book ofASTM Standards Vol 04.04, 4 Annual Book ofASTM Standards, Vol 09.01. 5 Annual Book ofASTM Standards* Val 06.01. 6 Annual Book ofASTM Standards, Vol 15.06. 7 Annual Book ofASTM Standards, Vol 08.01. R Annual Book ofASTM Standards, Vol 04.03. 9 Annual Book ofASTM Standards, Vol 15.09. 10 Annual Book ofASTM Standards, Vol 12.02. 11 Available from the Secretary, American Association of Textile Chemists and Colorists, P.O. Box 12215, Research Triangle Park, NC 27709. 1064 iJBiack-fi jpry Bii Hftelatlvl Specirr Rack S iSpecim fSpecim ' Ispedrr fidentify 13. S$ ,, 3.11 Jcondif dure [be spd practij weatbi 3.2!.,Igeogri may b : accord eqeilf tainM equiv|f degree* lishedj 3:3 r incuts^ among limits!' made.fc by the* I 4. Ap|i 41 I arc lay ,foIiow| the'ttE water? DUP050298242 Moratory . firaterial___ J 23 Test Method No. __ inference Standard Used: . tier ASTM Test No_____ Ixposure Apparatus: ASTM Type gifr Model - light Source: Enclosed _ Ijtere: Type .. lapsed Exposure Time: ixposure Conditions: Dark. glack-Panel Temperature Pry Bulb Temperature C (F) Relative Humidity " ecimen Water Spray Jack Spray {when used) __ * edmen Spray Water Type: tedmen Spray Nozzle Type: Mfg. Designation _ ecimen Relocation Procedure During Exposure: min . Method No. - Serial No.__ . Open Flame ----------- - Age Identify Properties to ba Determined on Test Specimens and identify Test Procedures or Methods Used for Property Measurement. Dperator/Oate: _____ ______ -______________________________________________________________________________________ *iupervisor/Date: --------------------------------------------------------------------!---------------------------------------------------------------------------------- - FIG. 1 Report Form 2.3 ISO Standard:*12 ISO Gray Scale 1 3. Significance and Use ,,r 3.1 Several types of apparatus with different exposure { ^conditions are available for use. No single operating proce dure for light exposure apparatus with or without water can i'be specified as a direct simulation of natural exposure. This 'practice does not imply expressly or otherwise an accelerated jweathering test. i | 3.2 Since natural environments vary with respect to [geography, topography, and different exposure periods, it | may be expected that the effects of natural exposure will vary [accordingly. Furthermore, all materials are not affected [equally by the same environment. Therefore, results ob tained by use of this practice should not be represented as `equivalent to those of any natural weathering test until the [degree ofquantitative correlation has been empirically estab lished for the material in question. 3.3 Variations in results may be expected among instru ments of different types and when operating conditions among similar type instruments vary within the accepted limits of this practice. Therefore, no reference should be made to results from use of this practice unless accompanied by the report form as specified in Fig. I. 4. Apparatus13 4.1 The apparatus employed shall use one or two carbon- arc lamps as the source of radiation, and shall be one of the following types, or equivalent. The term "cycle" is defined as the total time for all exposure conditions (light, light plus water spray, dark periods) that are repeated. n Available from American National Standards Institute. 1430 Broadway, New York. NY 10017. 13 Available from the Atlas Electric Devices Co., 4114 N. Ravenswood Ave., Chicago, IL. 606132 and from Suga Test Instruments Co., Ltd. 4-14, Shinjuku 5-chome, Shinjuku-ku, Tokyo, 160, Japan. No t ' 2--Several models of carbon-arc type exposure devices are no longer commercially available and should be considered obsolete. Exposures in these devices are not recommended and should only be made when mutually agreed upon by all interested parties. 4.1.1 Type D--Twin enclosed carbon-arc lamp apparatus, with a 762 mm (30 in.) diameter specimen drum rotating at 1 rpm, automatic control of temperature and cycle, and manually adjusted humidifier. 4.1.2 Type DH--Same as Type D, except with automatic control of the humidity. 4.1.3 Type E--Single open-flame sunshine carbon-arc lamp apparatus, with a 959 mm (37.75 in.) diameter specimen rack rotating at 1 rpm, automatic control of temperature and cycle, and manually adjusted humidifier. 4.1.4 Type EH--Same as Type E, except with automatic control of the humidity. 4.1.5 Type H--Single enclosed carbon-arc lamp appa ratus, with a 508 mm (20 in.) diameter specimen rack, rotating at 1 rpm, automatic control of temperature and cycle, and manual regulation of the humidity. 4.1.6 Type HH--Same as Type H, except with automatic control of the humidity. ...... 4.2 The apparatus should consist of a suitable frame within which is located a test chamber, and necessary com partments for housing control and regulating equipment. 4.3 Provision should be made for mounting or supporting the test specimens in a circular rack or drum that is rotated around the arc or arcs. This provides uniform distribution of , the radiation on all specimens around the circumference of the rack. It does not, however, improve the distribution of the radiation along the vertical axis. 4.4 Adequate ventilation should be provided in the test chamber to prevent contamination of the specimens from combustion products of the arc. 4.5 The apparatus should include equipment necessary for measuring and controlling the following: 4.5.1 Arc current, 4.5.2 Arc voltage, 4.5.3 Black-panel temperature (Note 3), 1065 f DUP0502 98243 # G 23 CT u "70 mm "1.5 mm FIG. 2 Black Panel Thermometer Unit Using Dial Type Thermometer with tire detailed requirements specified for the material tn ' be tested. 5.2 Mount the test specimens, except those whose s or other physical characteristics make it impractical, i rally both above and below the horizontal center line o! in,..; source of radiation. To assure that specimens receive thgfj greatest uniformity of radiant exposure, reposition nicm vertically in a sequence which will provide each specimen i equivalent exposure periods in each location. When the \ ' exposure interval does not exceed 24 h, each spec, nn u j should be located equidistant from the horizontal axis oi ihe arc. For exposure intervals not exceeding 100 h, daily! rotation of the specimens is recommended. Other methods ) of achieving uniform total irradiation may be employed ifs \ mutually agreed upon by concerned parties. I 5.3 For enclosed arcs only, where physical characteristics!t do not permit suspension ofspecimens iri a vertical position, 1 expose them horizontally on a rack 165 mm (6.5 in.) below ! the horizontal center of the source or sources of radiation. * Mount the specimens on a circular horizontal rack equipped with turntables, so that each specimen is rotated on its own axis as all ofthe specimens are rotated around the source or sources of radiation. 5.4 Temperature measurement and control should be based on the black-panel thermometer unit. Support the panel with the thermometer attached in the specimen drum* or rack in the same manner as the test specimens so that it will be subjected to the same influences, 4.5.4 Water-spray pressure, 4.5.5 Operating schedule or cycle, 4.5.6 Exposure time, and 4.5.7 Relative humidity {Types DH, EH, and HH only). 4.6 Types DH, EH, and HH apparatus are equipped with thermostatically actuated vaporizing units for adding mois ture to the air as it passes through the conditioning chamber prior to its entry into the test, chamber. Type H and some Types D, and E have manually regulated, electrically oper ated vaporizing units. Relative humidity of the air in the test chamber is calculated from the readings of the wet- and dry-bulb thermometers, either indicating or reporting, whose sensing portion is located in the air stream at its point ofexit from the test chamber. 4.7 The black-panel thermometer unit should consist of a stainless steel panel 1 by 70 by 150-mm (.060 by 2.75 by 5.875 in.) to which is mechanically fastened a temperature sensing device. This device shall be capable of measuring temperature to a repeatability of 4 1'C (see Figs. 2 and 3). The face of the panel with the temperature sensing device attached should be finished with two coats of baked-on black enamel selected for its resistance to light and water. 4.8 Detailed requirements and operating conditions ofthe apparatus are given in Table 1 and Figs. 4 to 6. appmcK, %!ishtm. fetiogr' inp% Jynlesb Jjippllitfc JJ|ioris,E,- A. 5.4 X ificatii.;J 5*F. 4, ' jbserf;.) 1.5 wn 5. General Procedure 5.1 Prepare specimens of a suitable size and shape for. mounting in the drum or rack ofthe apparatus in accordance FIG. 3 Black Panel Thermometer Unit Using RTD Thermocouple Sensor 1066 DUP050298244 al to men the men fthe laily tods :d if IlilP Q 23 TABLE 1 Detail Requirements and Operating Conditions of Light- and Water-Exposure Apparatus Type'* [he voltage, V: If 208 to 250 me voltage, V: 1120 to 145 148 to 52 3 current, A: IIS to 17. ac 158 to 62, ac 112 to 14, <Jc J 58 to 62, dc jarbon electrodes, upper: | neutral cored or solid | copper-coated sunshine pjarbon electrodes, lower: j neutral cored or solid copper-coated sunshine0 |lat panels of optical, heat-resistant glass with light transmission properties similar to Fig 7. #7740 Pyrex brand Filter panes (3.0 mm) typically will transmit 1 % at 278 nm, 5 % at 285 nm arid 50 % at 306 nm, #7058 Corex brand Filterpanes^ (2.5 mm) typically transmits 1 % at 252 nm, ;5 % at 262 nm and 50 % at 287 nm. iGlobe of optical, heat-resistant glass with nominal 1 % cut-off at 275 nm, with an increase in transmission to 91 % at 370 nm. , .. jpiameter of specimen rack or drum, mm (in.): 1 508(20) 762 (30) 960 (37.7) ppeed of rotation of specimen drum or rack: 1 rpm Automatic arc feed: Solenoid-operated Motor-operated iSpray (see figure indicated for arrangement, location, and capacity) D, OH X X X X X X X X Fig. 4 E, EH X Fig. 5 H, HH X X X X Fig. 6 4 "X" in column indicates application to that type of apparatus. 9 No. 70 Solid Carbon Electrodes and No. 20 Cored Carbon Electrodes or equivalent available from Atlas Electric Devices Co. or from Suga Test instruments Co., Ltd. 0 No, 22 Copper-Coated Sunshine Carbon Electrodes and No. 15.5 Copper-Coated Sunshine Carbon Electrodes or equivalent available from Atlas Electric Devices Co. por from Suga Test Instruments Co., Ltd. 0 No. 9200-PX Globe or equivalent. B 7740 Pyrex is a tradename for a soda borosiljcate glass. . . "I.1' F 7058 Corex is a tradename.for a potash lithia borosilipate glass. . r-., 5.4. 1 Program the instrument to operate in a continuous |!ight-on mode. Fill specimen rack with blanks and the Iblack-panel thermometer. Operate in this mode while estab- flishing the black-panel temperature according to the manu- ' Jfacturer's instructions. Allow the machine to come to oper- iating temperature and equilibrate, (allow 4 h rif continuous punning time and between 25 to 35 min after a spray cycle). Ipnless other temperatures and tolerances are specified in the japplicable ASTM test method or detailed material specifica- Itions, the black-panel temperature shall be 63 " 2.5C (145 |5T) (Note 3). ' ' 5.4.2 Compare the black-panel temperature with the spec ification. If the black-panel temperature is within 2.5 C or |5F of specification, no adjustment is necessary. If the I observed temperature difference is greater than 2.5C or 5F, | adjust the temperature controller and recheck the black- | panel temperature during the next cycle. It is recommended p that this : procedure be performed. after every 200 h of l machine operation. No t ' 3--Where desired, othec black-panel temperatures may be I employed provided they are specifically noted in the report of test I results. Instructions for adjusting the intensity of the arc and the fading * rate are supplied with the apparatus or are available upon request from the manufacturer. Consideration should always be given to installing the J instrument in a room where the temperature arid humidity conditions i are controlled. The magnitude of the effects due to variation in the air supply can only be partially determined when the intake air is not controlled. .5.5 The water from the specimen spray should strike the test specimens in the form, of a fine spray equally distributed over the test specimens. Unless otherwise specified in the applicable ASTM test method or detailed material specifica tion, the waier pressure, number, and type of nozzles should' be in accordance with the detailed requirements for the various types of apparatus as indicated in Figs. 4 to 6. The pH of the water shall be 6.0 to 8.0, contain less than 1 ppm solids and leave no, objeptional deposits or stain on the specimens.' The'presence of very Idw levels of silicates in spray water has been shown to leave deposits on some specimens. If is recommended that the temperature of the water should be 16 5 'C (60 9"F), Recirculation is not recommended and must not be done unless the recirculated water is treated to meet the above requirements. 5.5.1 Set the cycle control unit cam until the machine is in a spray cycle. Observe the spray manifold. All spray heads should spray a stream of mist or water which reaches the panel surface. If any of the spray heads are not satisfactory, remove the spray manifold and clean each spray head. Install the manifold and recheck the spray operation. 5.6 The flat glass filter panes used in Types E or EH devices cannot be used for more than 2000 h. Monitor age and position of the filter panes so that the oldest can be 1067 DUP050298245 # G 23 WPSNIPOINTETZHCSZIML4OEEFNNPOWSRZAPEZTRSLEASERTUSRPUEEONRPITEOMREfIAQN1TUU2EiTOFETPOSAFOTR1OA8MP3li NO.SO NOZ ZLE - 4A TO 5.3 PINTS/MIN h. 1 vs Metric Equivalents mm 3.3 34.9 92.1 101.6 293.2 762 83 to 124 kPa in. Ve . 1% 36/s 4 11Vie 30 12 to'18-psi FIG. 4 Specimen Spray Arrangement for Types D and DH'Apparattis. removed every 250 h. Filter globes used in type D or DH devices cannot be used for more than 2000 h. Replace the oldest of the filter globes every 1000 hi Replace the filter globe in Type H or HH devices after 2000 h of use or when pronounced discoloration or milkiness develops. Clean filters each day by wiping, with a clean, dry non-abrasive cloth or towel. Filters can also be cleaned by washing with water, or a solution of detergent and water. 5.7 Unless otherwise specified in the applicable ASTM test method or detailed material specifications, operate Types E and EH apparatus with the filters in place' and with the carbon electrodes specified in Table 1. If operated without filters or with other types ofcarbon electrodes, state this in the report of test results. METHOD 1--CONTINUOUS EXPOSURE TO LIGHT AND INTERMITTENT EXPOSURE TO WATER SPRAY 6. Apparatus 6.1 The apparatus may be any of the recommended type equipped with water spray nozzles. 6.2 Program the instrument for continuous light and intermittent water spray according to the manufacturer's instructions. Since there are numerous light and water spray cycles which can be used, the cycle program selected must be by mutual agreement among the interested parties. Histor ical convention has established a cycle Of 102 min of light followed by 18 min of light and water spray. This. cycle permits the attainment ofthe maximum black-panel temper* attire during the light only portion of`the exposure. 6.2.1 When testing the effects of photodegradation only, the water spray may be omitted (refer to Method 3)'. 6.3*In Types DH, EH and HH apparatus, dry and wet bulb temperature controls, humidifier and immersion heater controls should be adjusted as specified. 6.4 In Type H and in Types D and E with humidifier, humidity may be adjusted but not controlled. METHOD 2--ALTERNATIVE EXPOSURE TO LIGHT AND DARKNESS AND INTERMITTENT EXPOSURE TO WATER SPRAY 7. Apparatus 7.1 The apparatus shall be Type DH, EH and HH apparatus with automatic humidity control and water spray nozzles. 7.2 Operation during the light on period should be as described in Section 5. 1068 parat#> expo!;; 7.3 ;; ay be!' Br f I: DUP050298246 G 23 mm 101.6 117.5 136.5 266.7 959 in. 4 4Ve 53/g 10V2 37% 124 to 172|<Pa 18 to 25 psl 0.26 to 0.36 dm3 0.46 to 0.64 pt FIG. 5 Specimen Spray Arrangement tor Types E and EH Single Open-Flame Sunshine Carbon-Arc Lamp Apparatus 7.2.1 Separate controls for temperatures and humidificajon may be adjusted during the dark period for automatic control as. the cycle alternates from light to dark. In Type EH pparatus, a spray rack to cool the specimens by wetting the nexposed back surface can result in development of conlensation on the exposed specimen surface during the dark interval. 7.3 All Types DH, EH, H, HH and some Type D, and E ay be programmed to operate with alternating light and lark intervals without control of relative humidity. METHOD 3--CONTINUOUS EXPOSURE TO LIGHT WITHOUT WATER SPRAY Apparatus 8.1 The apparatus shall be Type D or DH, E or EH, H or 1H light-exposure devices programmed for continuous light bnly, according to the manufacturer's instructions. 8.2 Adjust the controls on the apparatus so that the black aiiel temperature is 63 2.5C (145 5F) (Note 3), and for a relative humidity of 30 5 % in devices with automatic humidity control. 8.-3 Expose the materials to -be tested as determined by mutual agreement among the concerned parties or, when not otherwise'specified, in accordance with one of the following: 8.3.1 Versus One AA TCCBlue Wopl Lightfastness Stand ard--Expose the test specimen and any mutually agreed upon AATCC Blue Wool Lightfastness Standard partially masked until the difference between its masked and un masked portion exhibits a color change equal to Step 4 of the ISO Gray Scale. Report the results by any mutually agreedupon method of measuring change in the test specimen. 8.3.2 Versus Set of AATCC Blue Wool Lightfastness Standards--Expose the test specimen and a set of AATCC Blue Wool Lightfastness Standards partially masked until a maximum permissible amount of change, as determined by specified or mutually agreed-upon method of measurement, occurs in the test specimen. Assign it a classification number equal to that of the numbered standard that most nearly exhibits a change in color equal to Step 4 on the ISO Gray Scale. Where one standard shows a color change greater than Step 4 and the next higher number standard shows less than a Step 4 color change, an intermediate or half-grade rating may be used. 1069 DUP0502 98247 # G 23 #7058 CorexA l?.5 mn) % TRANSMITTANCE #7740 Pyrex8 FIG. 7 Representative UV Transmission Curves for 2.5 mm and 3 mm Filter Grasses'4 A # 7058 Corex is.a tradename for a potash litftla borosilicate glass. B #7740 Pyrex is a tradename for a soda faorosilicate glass. 3.2 mm 38.1 mm 76.2 mm 88.9 mm 508 mm 34 to 55 kPa 0.66 to 0.73 dm3 '/e in. 1 Vz in. 3 in. 3'h in. 20 in. 5 to 8 psi 1.0 to 1.3 pt FIG. 6 Specimen Spray Arrangement for Types H and HH Single Enclosed Carbon-Arc Lamp Apparatus 8.3.3 Versus Other Standard Sample--Expose the test specimen and any mutually agreed-upon standard sample until either shows an agreed-upon amount of change when measured by any mutually agreed-upon.method. Report the results on the basis of a comparison of the specimen with the standard sample. METHOD 4--ALTERNATE EXPOSURE TO LIGHT AND DARKNESS WITHOUT WATER SPRAY9 9. Apparatus 9.1 The apparatus shall be Type H or HH programmed to a predetermined cycle of light and darkness by turning off the carbon arc. 9.2 The procedure for Method 4 is the same as specified for Method 3 except that the following light-dark interval shall replace the continuous light condition of Method 3. 9.2.1 Unless otherwise specified by the detailed require ments for the type of material being tested, adjust the controls ofthe apparatus so that it produces a cycle of 1 h of darkness followed by 3.8 h of light Repeat this cycle for the duration of the test. During the light-on period the blackpanel temperature, at equilibrium, shall be 63 2.5C (145 5F). During the period while the light is off, the black-panel temperature will progressively drop until it is in equilibrium with the air in the test chamber. The relative humidity of the air at the face of the test specimens will progressively rise during the light-off period until equilib rium is reached. 10. Report 10.1 The report shall include the following: 10.1.1 Type and model of exposure device, 10.1.2 Type of light source, 10.1.3 Type, thickness, and age of filters, 10.1.4 Elapsed exposure time, 10.1.5 Light and dark-water-humidity cycle employed, 10.1.6 Operating black-panel temperature, 10.1.7 Operating relative humidity, 10.1.8 Type of spray water, 10.1.9 Type of spray nozzle, and 10.1.10 Specimen relocation procedure. APPENDIX (Nonmandatory Information) XI. OBSOLETE APPARATUS Xl.l The following types of apparatus are no longer commercially available and should be considered obsolete. Although existing units may be operated in accordance with Methods 1 and 3 of this practice, results may not be comparable with those obtained in superseding models. X1.1.1 Type A--Single enclosed carbon-arc lamp apparatus* 1070 DUP050298248 ind 3 # G 23 with a 762 mm (30 in.) diameter specimen drum rotating at I rpm, automatic control of temperature and cycle, and no BS Automatic control of the humidity. Jr ' XI. 1.2 Type AH--Same as Type A, except with autol^iftatic control of humidity. XI. 1.3 Type B--Single enclosed carbon-arc lamp appa|atus, 3 RPH, 762 mm (30 in.) diameter specimen drum, Automatic temperature control, no automatic humidity con trol. Last manufactured in 1955. X1.1.4 Type C--Same as Type B but without automatic temperature control. Last manufactured in 1960. XL 1.5 Type F--Single open flame carbon arc lamp apparatus, 0.5 rph, 960 mm (37.75 in.) diameter specimen rack with vertical specimen mounting. No automatic control of temperature or humidity. Last manufactured in 1950. Xl.1.6 Type G--Same as Type F but with inclined specimen rack: The American Society for Testing end Materials lakes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination oi the validity of any such patent rights, and the risk of infringement of such rights, are entirety their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and itnot revised, either reepproved or withdrawn. Your comments are invited either lor revision otthis standard or lor additionalstandards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should mate your views known to We ASTM Committee on Standards, 1916 Race St, Philadelphia, PA 19103. ified :rval ure- the h of the ick- 145 the s in tive will 91 .lib- 1 1071 DUP050298249 Designation: G 26 - 90 Standard Practice for Operating Light-Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of Nonmetaiiic Materials1 This standard is issued under the fixed designation G 26; the number immediately following the designation indicates the year df original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. P superscript epsilon (<) indicates an editorial change since the last revision or reapproval. I. Scope 1.1 This practice covers the basic principles and operating procedure for water- or light-exposure apparatus, or both, employing a xenon-arc light source. Non I --This practice combines the practices previously referred to as G 26 and G 27. Practice G 27, for Operating Xenon-Arc Type Apparatus for Light Exposure of Nonmetaiiic Materials*, has been discontinued since it is now covered in this edition of G 26 under Test Methods C and D. 1.2 This practice does not specify the exposure conditions best suited for the material to be tested, but is limited to the method of obtaining, measuring, and controlling the condi tions and procedures of the exposure. Sample preparation, test conditions, and evaluation of results are covered in ASTM methods or specifications for specific materials. i .3 This practice includes four test methods: 1.3.1 Test Method 1--Continuous exposure to light and intermittent exposure to water spray. 1.3.2 Test Method 2--Alternate exposure to light and darkness and intermittent exposure to water spray. 1.3.3 Test Method 3--Continuous exposure to light without water spray. Exposure conditions are characteristic of those specified by AATCC Test Method 16E 1976. 1.3.4 Test Method 4--Alternate exposure to light and darkness without water spray. Exposure conditions charac teristic of those natural conditions experienced when ex posing are in accordance with Practice G 24. 1.4 This practice may involve hazardous operations and equipment. Thispractice does not purport to address all ofthe safety problems associated with its use. It is the responsibility ofthe user ofthis practice to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. 1.5 The values stated in SI units are to be regarded as the standard. The inch-pound equivalents of the SI units may be approximate. 2. Referenced Documents 2.1 ASTM Standard: G24 Practice for Conducting Natural Light Exposures Under Glass2 2.2 AA TCC Standard: Method 16E 1976 Colorfastness to Light, \\ di*r-C('ulw' Xenon-Arc Lamp Continuous Light3 2.3 CIE Standard: fg| No. 20 Recommendations for the Integrated Tt t S' M and the Spectral Distribution of Simulated Sol, rV'iW'4! tion for Testing Purposes4 2.4 ISO Standard: am' Gray Scale 3. Significance and Use 3.1 Several types of apparatus with different exfickB., conditions are available for use. No single ope.atTa^rgjiS dure for light-exposure apparatus with and with jut be specified as a direct simulation of natural expmrmatl practice does not imply expressly or otherwise an ariSra**" weathering test. *9jSgB 3.2 Since the natural environment varies with evpV""'-`il,'*! time, geography, and topography, it may be expected the effects of natural exposure will vary accordingly. 'l||j rials are not affected equally by the same cnuronqjctyd Results obtained by use of this practice should 'n<jf'?!b$5 represented as equivalent to those of any natur.d vtoatheifmgS test until the degree of quantitative correlatiui has b!'* established for the material in question. 'Vitf 1. 3.3 Variations in results may be expected amo ig i'lstffk ments of different types or when operating conditions amt1 2 similar type instruments vary within the accepted Ji Saits',* this practice. Therefore, no reference should be results from use of this practice unless accompa^ed by' ' report form shown in Fig. 1 or unless otherwise p-- iJitd'ifi referenced procedure. jjH 4. Apparatus 4.1 Water-Cooled Type:5 4.1.1 The apparatus employed should utilize a v^fgggL cooled xenon-arc lamp as the source of radiation and snouJiLi be one of the following general types, or their equr aleHbjjB 4.1.1.1 Type A--An exposure apparatus in w 'ick.t.iNS-j source of radiant energy shall be a water-cooled At-neP.-ahL, vertically located at the central axis of either a SOs-pSra (20-in.) diameter vertical specimen rack, or of a 548j0gj||l (25.5-in.) diameter inclined rack. Means shall be provT for automatic programming of temperature and ejcl^ i.TO My- 1 This practice is under the jurisdiction of ASTM Committee G-3 on Durability of Nonmetaiiic Materials and is the direct responsibility ofSubcommittee G03.03 on Simulated and Controlled Environmental Tests. Current edition approved Jan. 26, 1990. Published March 1990. Originally published as E239-64T. Redesignated G 26 in 1970. Last previous edition G 26 - 88<l. 2 Annua! Book ofASTM Standards, Vo! 14.02. 3 Available from The Secretary, American Association of Textile Cheml^l Colorists, P.O. Box 12215, Research Triangle Park, NC 27709. 4 Available from Secretary, U.S. National Committee, CIE, National of Standards and Technology, Gaithersburg, MD 20899. 5 Available from Atlas Electric Devices Co., 4114 N. Ravenswood, Chicago, IL 60613. 1072 ' DUP050298250 # G 26 Cooled idiance Radia- posure procetercan 5. This erated >ect to latthe matetnent, ot be lering been nstrumong its of de to iy the din a laboratory . Material. G 26 Test Method No. __ reference Standard Used: Ither ASTMTest No.,, . Method No. Exposure Apparatus: ASTM Type ___ ________________ Mfr. Mode!__Serial No. i jjght Source: Water-Cooled____W. Air-Cooled___ Jethod Used to Regulate Wattage to Lamp __________ `Optical Filters: Type------------------------- ;----- - Age------- Spectral Irradiance:W/m at Jfifadiatlon Units:AJ/m2 How Monitored: _ Elapsed Exposure Time:h Exposure Conditions: Program_____ Lighti Dark - Black-Panel Temperature --C<*F) Air Temperature -- C (*F) `Dry Bulb Temperature --_UC (F) g., Relative Humidity __ * Specimen Water Spray __ min cycle Specimen Nonspray __ min cycle pspecimen Spray Water Type: --------- I*Spec&nen Spray Nozzle Type: Mfg. Designation - ^Specimen Relocation Procedure Ouring Exposure: __ 0C<F) __% _,m'n cycle __ min cycle lilentify properties to be determined on test specimens and identify test procedures or methods used for property measurement. pperator/Date: _ Supervisor/Date; ICompany: _____ FIG. 1 Report Form iMeans shall be provided for adjustment of relative humidity. |The specimen rack shall rotate at 1 0.1 rpm. N' 2--In the commercial descriptions of the four types, the term |t``cycle" is defined as each time interval of light, darkness, and water jispray that is specified differently in accordance with the different testing Imethods. 4.1.1.2 Type AH--The exposure apparatus shall be idenitical to Type A except it shall have automatic humidity ficontrol. 4.1.1.3 Type B--An exposure apparatus in which the I source of radiant energy shall be a water-cooled xenon-are II vertically located at the central axis of a 960-mm (37.75-in.) 1 diameter specimen rack. Means shall be provided1 for auto- K matic programming of temperature and cycles. Means may 1 be provided for adjustment of humidity. The specimen rack I shall rotate at 1 0.1 rpm. 4.1.1.4 Type BH--The exposure apparatus shall be sim ilar to Type B except it shall have automatic humidity j control. 4.1.2 The xenon-arcs employed shall be of the "long arc" j water-cooled type operated through suitable reactance trans(formers and electrical equipment from a 50 or 60-Hz power I supply. They shall employ cylindrical inner and outer optical f filters to direct the flow of cooling water and to simulate.a designed spectral energy distribution. 4.1.2.1 For the purpose of this practice, the xenon-arc lamp shall consist of a quartz xenon burlier tube and one of the following optical filter combinations:6-7 fl Norton, Kiuntke, and Connor, Canadian Textile Journal, CTJOA, May 1969. 7 Corning 7740 Pyrex (borosilicate), Coming 460! 1R absorbing visible transmitting, Kimble R6 soda lime glass tubing, and General Electric QA-204 quartz tubing of proper dimensions have been found suitable for use as xenon-arc optica] filters Available from Atlas Electric Devices Co., 4114 N. Ravenswood Ave., Chicago, IL 60613. (a) Borosilicate glass inner and outer optical filter to simulate the spectral power distribution (SPD) of natural daylight throughout the actinic region. lb) Infrared absorbing glass inner optical filter with quartz outer optical filter to simulate the SPD of natural daylight (300 to 1000 nm). (c) Borosilicate glass inner optical filter with soda lime glass outer optical filter to simulate the SPD of natural daylight (actinic wavelengths) filtered through window glass. (d) Infrared absorbing glass inner and outer optical filter to simulate the SPD of natural'daylight (310 to 1000 nm) filtered through window glass. (e) Quartz inner and outer optical filter to approximate sunlight intensities unfiltered by the earth's atmosphere.6 7 4.1.2.2 To prevent loss in levels of irradiance due to excessive solarization .and to .prevent possible breakage caused by stresses in optical filters exposed to high-intensity UV energy, inner optical filters8 shall be replaced periodi cally. Suggested intervals are 300 and 400 h for Types A and B, respectively. The outer optical filter shall be replaced after 1500 and 2000 h for Types A and B, respectively. 4.1.3 Distilled or deionized water should be recirculated past the burner at a flow rate sufficient to remove excess heat. Passing water through a cartridge demineralizer in stalled in the recirculation line just ahead of the lamp minimizes contamination of the quartz envelope of the burner. A heat-exchange unit should be used to cool the recirculated lamp water. 4.1.4 Since xenon-arc lamps, like all gas discharge lamps, will have a progressive drop in radiation output with continued use, and since optical filters will change in their 8 Kishii, T., and Ooka, K., Symposium on Coloured Glasses. International Comm, on Glass of Czech. Sci. & Tccli. Soc. of the Silicate Industry, 1967. 1073 DUP050298251 ffi G 26 transmission characteristics, provision shall be made in the apparatus (automatically or manually) for progressively in creasing the wattage of the lamp to minimize changes in the intensity of the radiation at the face of the sample. The greatest change in both the xenon burner tube and optical filters occurs in the first 20 h of use. For this reason, burners and optical filters preaged by the instrument manufacturer are recommended for critical testing when a more rapidly changing rate of intensity is undesirable. For routine testing on a comparative basis, the 20 h of preaging may be omitted. 4.1.5 Many nonmetallic materials are selectively ab sorbing. The energy that a molecule absorbs depends upon the wavelength of the incident radiation.9 It is desirable to monitor the level of irradiance of the photochemically effective wavelengths if intercomparisons are to be made among samples not exposed simultaneously. Samples may then be exposed to known amounts of irradiation, the time integral of irradiance. 4.1.5.1 Where radiometers capable of monitoring discrete portions of a continuous spectrum are available, exposure to a mutually agreed-upon level of irradiation may be specified as the exposure interval in place of a time interval. {a) When using the optical filter combination described in 4.1.2.1 (a), the suggested minimum spectral irradiance levels are: .2 W/m2/nm band at 320 nm ,35 W/mVnm bancbat 340 nm ' , .5 , W7m2/nm band at 380 nm . .75 W/m2/nm band at 420 nm. . . (6) When using the optical filter combination described in 4. i .2.1 (c), the suggested minimum spectral irradiance levels are: ' ' .2 W/m2/nm band at 340 nm .45 W/m2/nnt band at 380 nm .7 W/m2/nm band at 420 nm (c) Operating at the suggested minimum' levels approxi mates the average daily solar irradiance under ideal condi tions. It is about half of the maximum values for total irradiance on a Horizontal plane when the sun is at 90" altitude as reported in CIE No. 20. When irradiance is monitored and periodic manual adjustment of wattage is made to compensate for changes of intensity, no lamp assembly should be used that cannot maintain the minimum level of irradiance within a 10 % tolerance at the monitored wavelength, irradiation expressed as joules per square metre is the product of irradiance x exposure time in seconds. 4.1.5.2 Xenon-arc type equipment not having a radiom eter shall be operated with periodic increases in wattage to minimize any drift in levels of irradiation. Such intervals shall be established by the parties concerned or follow the suggested schedule below in 4.1.5.2 (a). N' 3--The use of suggested wattage steps does not imply that irradiance will be maintained at levels equivalent to those obtained when employing a light monitor. They are intended as a guide to minimize the reduction of UV intensity with maximum lamp longevity when using either Test Method A or C for 2.5, 6, or 6.5-kW lamps, respectively. 'Hawkins, W.L., ed., "Polymer Stabilization," Wiley-lniersdence, 1972. p. 166. (a) The following are the suggested wattage settings* each exposure interval of a 2500-W xenon burner tube b upon the average performance of xenon burner tubes borosilicate filters: Time, h Oto 20 20 :o 200 200 to 400 400 to 600 600 to 800 800 to 1000 1000 to 1200 1200 to 1500 Power, W 1600 1800 2000 2250 2500 '2600 2800cr 3000 -ifllgP (b) The following are the suggested wattage Settings for ! each exposure interval of a 6000-W xenon burner tube based! upon the performance of xenon burner tubes with boiosili-1 cate filters in Test Method A: Time, h Ppwer, W Oto 20 20 to 100 100 to 250 250fo 400 400 to 550 550 to 700 700 to 850 850 to 1000 min 4750 5000 5250 5500 6000 6500 7000 (c) The following are the suggested wattage settings for . each exposure interval of a 6500-W xenon burner tube based f upon, the average performance of xenon burner tubes, with* borosilicate filters in Test Method A: - Time, ft . Pov^er, W , O to 20 20 to 100 100 to 200 200 to 500 . 500 to 1000 1000 to 1500 1500 to 2000 " ' 2000 and over ' min 5500 6000 6200 6500 ' 7000 7500 8500 4.1.6 Specimens should be mtmnted on a rack rotating about the, lamp at a 'diStaiice such that the location of each specimen assures that the irf&diance incident on its surface does not'vary by more than 5 % from the average. Figure'4 illustrates'a rack meeting this condition. '4.1.7 Any apparatus--that does hot comply with the condition of 4.1.6 shall not have a variation in irradiance exceeding 10 % of the average, and may require specimen rearrangement during exposure, in accordance with the test procedure, in order to minimize the variability in radiant exposure. 4.1.8 Testing temperatures should be'measured and regu lated on the basis of a black panel thermometer unit mounted on the specimen rack so that the face of the unit is in the same relative position and is subjected to the same influences as the test specimens. The black panel thermom eter unit should consist of a .stainless steel panel about 70 by 50 by 0.95 mm (2.750 by 5,875 by 0.0375 in.), to which a stainless steel bimetallic dial-type thermometer is mechani cally fastened. This thermometer should have a stem approx imately 4 mm (0.16 in.) in diameter with a 44.5-ram {1.75-in.) dial. The sensitive portion extending about 38 mm (1.5 in.) from the end of the stem should be located in the center of the panel approximately`64 mm (2.5 in.) from the top and approximately 48 mm (1.875 in.) from the bottom ! tb| . 1074 DUP050298252 G 26 i for asecT; with for ased isili- for ised vith -ing ach ' ace e4 .the nee aen. test' ant gu-. init t is me mby 5a ni- 3X- im lm the the if the panel. The face of the panel with the thermometer :em attached should be finished with a baked-on black infrared-absorbing coating having good resistance to light. 4.1.8.1 A thermocouple or resistance bulb thermometer ounted at the center face of the black panel, which rovides temperature values equivalent to the dial tkermom- iter, may be substituted. 4.1.9 A blower unit in the base of the apparatus should provide a flow of air through the test chamber and over the test specimens. Control ofspecimen and black-panel tempertture should be accomplished by thermostatic control of the temperature of the constant volume of air from the blower, lack-panel temperatures should be read through the fvindow in the test chamber door without opening the door. 4.1.10 Apparatus operated as a light- and water-exposure st shall be equipped with a specimen spray unit as illusated in Figs. 2 and 3. All components of the specimen spray ||mit should be fabricated from stainless steel, plastic, or other Bmaterial that does not contaminate the water. Apparatus operjjated orily as a light-exposure test are not required to have the Bspecimen spray unit or, if present, it should not be used. If 4.1.11 Types A, AH, BH, and some Type B apparatus are ' equipped with an electrically operated vaporizing unit for padding moisture to the air as it passes through the condi. tioning chamber in the base section prior to its entry into the itest chamber of the apparatus. ' 4.1.11.1 In Types A and B, the vaporizing unit, when I manually turned on, may operate continuously while the apparatus is in operation. Type A and some Type B apparatus may be programmed to operate the vaporizer [during a dark cycle only. The temperature of the water, with (which the vaporizer is supplied, is not controlled. In Type B ^apparatus not supplied with a vaporizing unit, the relative humidity within the test chamber is governed by evaporation % of water in the bottom of the chamber and from water i emitted through the specimen spray unit.. 4.1.11.2 In Types AH and BH apparatus, operation of the vaporizer is controlled automatically by a wet-bulb thermo stat. The temperature of the water supplied to the vaporizer ; is regulated automatically by thermostatically-actuated elec- [ trie immersion heaters. Control automatically shifts between ^ two separate sets of thermostats as the arc lamp is turned on ' and off by the program control unit. 4.1.12 In Types A, B, AH, and BH apparatus containing vaporizing units, relative humidity is determined from wet| and dry-bulb thermometers located in the air stream at the 5 vaporizer's point of exit from the test chamber. | 4.1.12.1 Determine the relative humidity for Type B I apparatus not equipped with a vaporizing unit from wet- and 4 dry-bulb thermometers mounted in holders on the specimen rack so that their sensitive portions are in the same relative position as the face of the test specimen but shielded from the radiation. 4.1.12.2 Any apparatus with a vaporizing unit operated with the unit and immersion heaters turned off will provide essentially the same conditions of relative humidity as are produced in Type B apparatus without a vaporizing unit. 4.1.13 The apparatus shall include means for measuring the following: 4.1.13.1 Wattage of the xenon-arc lamp, 4.1.13.2 Irradiance at the specimen rack, 4.1.13.3 Black-panel temperature, 4.1.13.4 Dry-bulb temperature (test chamber), 4.1.13.5 Wet-bulb temperature (test chamber), 4.1.13.6 Exposure interval, and 4.1.13.7 Water spray pressure when applicable. 4.1.14 Where specified, the apparatus shall include means for regulating or controlling the following: 4.1.14.1 Wattage of the xenon lamp, 4.1.14.2 Irradiance or irradiation, or both, at the spec imen rack, 4.1.14.3 Temperature (test.chamber), 4.1.14.4 Relative humidity (test chamber), 4.1.14.5 Light-dark-spray-humidity-temperature cycles, and 4.1.14.6 Water spray pressure when applicable. 4.2 Air-Cooled Type:10 4.2.1 The apparatus employed shall use an air-cooled xenon-arc lamp as the source of radiation and should be one of the following types, or their equivalent: 4.2.1.1 Type C--Air-cooled xenon-arc apparatus, 1500 W, 158-mm (6.2-in.) diameter specimen rack, with auto matic programming of cycles and humidity. The specimen rack should rotate at 5.2 0.1 rpm. 4.2.1.2 Type D--Air-cooled xenon-arc apparatus, 4500 W, 360-mm (14.2-in.) diameter specimen rack, with auto matic programming of temperature, cycles, and humidity. The specimen rack should rotate at 3.7 0.1 rpm. 4.2.1.3 Type E--Air-cooled xenon-arc apparatus, three lamps operating simultaneously at 4500 W each, 610-mm (24.1-in.) diameter specimen rack, with automatic program ming of temperature, cycles, and humidity. The specimen tack should rotate at 2.0 0.1 rpm. 4.2.2 The xenon arcs employed in Types C and D should be of the medium-pressure, air-cooled type and one or more optical filters shall be fitted between the light source and the samples to filter out undesired wavelengths of radiation. A combination of optical filters recommended by the manufac turer shall be used to simulate (/) sunlight in the open, (2) sunlight behind window glass, or (5) any other simulated solar irradiation condition desired. 4.2.3 All gas discharge lamps have a progressive_drop in radiant output with continued use. For Types C and D, it is recommended to exchangrthe IR-optical filters for new ones after 3500 h of use. Answering the purpose, not all seven IR-optical filters of the filter lantern should be exchanged at the same time but each should be exchanged after it has been running for 3500 h. For Type E which has three lamps, one lamp should be replaced every 500 hours to minimize the overall drop in radiant output. For Type E, the three partial preaged filters should be cleaned monthly and replaced after five years of normal usage. 4.2.4 Specimen holders should rotate around the arc, describing a cylindrical surface, so that specimens may face, or be turned opposite to, the arc. No part of the specimens shall be above or below the ends of the arc. Repositioning of specimens in upper, center, or lower positions can improve the uniformity of intensity of the exposure. 10 Available from DSET Labs, Box 1850. Black Canyon Stage I. Phoenix, AZ 85027. 1075 DUP050298253 # G 26 PINTS (LITERS) OF WATER PER MINUTE FOR SPECIMEN SPRAY UNIT EQUJPTED W7H 2 NOZZLES OPERATED AT A PRESSURE 0F> 18*25 P.S.I. (124-172 kPc) F-80 NOZZLE AT 0.23 TO 0.32 PINT5/MIN. (0.109 TO 0.152 UTERS/MINUTE) Metric equivalents 2% in. 4 in. 20 in. 18psi 25 psi 0.23 pt 0.32 pt 60.325 mm 101.6 mm 508 mm 124 kPa 172 kPa 0.109 liter 0.152 liter FIG. 2 Specimen Spray Arrangement for Type A and AH Apparatus 4.2.5 Testing temperatures should be measured and regu lated on the basis of a black-panel thermometer unit that is mounted so that the face of the unit is in the same relative position and is subjected to the same influences as the test specimens. The black-panel thermometer unit should consist of a stainless steel panel approximately 48 by 200 by 1 mm (1.9 by 8.0 by 0.04 in.), to which a stainless steel bimetallic dial-type thermometer is mechanically fastened. The temper- 1076 DUP050298254 PINTS (LITERS) OF WATER PER MINUTE FOR SPECIMEN SPRAY UNIT EQUIP7ED WITH 4 NOZZLES OPERATED AT A PRESSURE OF 18-25 P.S.1. (124--172 KPo) AT 0.40 TO 0.64 PINTS PER MINUTE <0.218 TO 0.304 LlTERS/MINUTD F-60 SPRAY NOZZLE ----- 4' (101.B mm) I ik ----- S 3/S (136.5 mm) - 4* (101.6 mm) r 4 in. 4% In. 5Ve in. 1OVfe in. 37y< in. 101.6 mm 117.48 mm 136.52 mm 266.7 mm 95B.85 mm fl Metric Equivalents 18psi 25 psi 0.46 pi 0.64 pt 124 kPa 172 kPa 0.218 liter 0.304 liter FIG. 3 Specimen Spray Arrangement for Type B and BH Apparatus d consist >y 1 mm imetallic temper- .ture at the center of the panel should be sensed by_the thermometer. The face of the panel should be finished with a >:baked-on black glossy enamel having good stability to light. 4.2.6 A blower unit in the base of the apparatus shall provide a flow of air through the test chamber and over the test specimens. Control of the specimen and the black-panel temperature should be accomplished by thermostatic control of the temperature of the constant volume of air from the blower. Black-panel temperature should be read through the ^window in the test chamber door without opening the door. 4.2.7 The apparatus should be equipped with a system to spray the specimens uniformly with water. This system should be of stainless steel, plastic, or other material that does not react with or contaminate the water employed. 4.2.8 Relative humidity in the test chamber should be measured and controlled by a contact hygrometer. Water should be vaporized and diffused to enrich the air with moisture and produce the required humidity. 4.2.9 The apparatus shall include equipment necessary for measuring and controlling the same parameters as listed for water-cooled xenon arcs. 1077 * i. it 1 DUP050298255 G 26 I 5. General Procedure 5. L Check to be sure the apparatus is operating properly at the start of each test. Check the lamp operation at 100-h intervals to be sure the burner tube and optical filters are dean and that they have not exceeded the maximum recommended period of use. 5.2 Program the instrument to operate in the continuous light-on mode without water spray. Fill the specimen rack with blanks and the black-panel thermometer. Operate the instrument in this mode while regulating the chamber dry-bulb temperature to provide the desired black-panel temperature of 63 3C (145 5F). 5.3 When the chamber dry-bulb temperature has been regulated, adjust instruments with automatic humidity con trol to the desired relative humidity (Types C, D, and E) or to the chamber wet-bulb temperature (Types A and B) at the level that will ensure the desired relative humidity. 5.4 In Types A, B, C, D, and E apparatus, use the type and iiumber of spray nozzles (Figs. 2 and 3) recommended by the manufacturer and operate at a pressure of 124 to 172 kPa (18 to 25 psi), measured at the nozzle unless otherwise recommended. The water shall have a pH of 6.0 to 8.0, contain less than 20 ppm solids, and leave no deposit or stain on the specimens after continued exposure in the apparatus. The temperature of the water should be 16 + 5C (60.8 9F), and recirculation of the water shall not be permitted . unless the recirculated water meets the above requirements. Pass the specimens through the spray once in each minute or revolution ofthe rack during the spray cycle. Allow the water to strike the test specimens in the f6rm ofa fine spray equally distributed over the specimens. 5.5 The temperature of the rack spray water should be sufficiently low to reduce the specimen temperature below the dewpoint when the specimen is continuously sprayed during a dark cycle. 5.6 Reference Standards: 5.6.1 AATCC Blue Wool Lightfastness Standards.3 N' 4--The eight standards L-2 to L-9 have been made by blending wool dyed with the fugitive dye Erio Chrome Azuroie B and wool dyed with the fast dye Indigosol Blue AGG in different propor tions. The blended wools were spun into yarns and the yarns woven into cloths. Each standard is approximately twice as fast as the next lower numbered standard. It has been found that when new lots of the standards are produced, the amounts of .the dyes required and tire properties of the two wools in the blends are often different from those used originally. The dyeing strengths and blending proportions would therefore be misleading, and they are intentionally not specified. 5.6.2 Any standard sample established by mutual agree ment between the purchaser and the supplier. 5.6.3 ISO Gray Scale for Assessing Change in Color.n 5.7 When the material to be evaluated is suspected of being very sensitive to variations in radiant exposure, and the apparatus does not meet the requirement of 4.1.6, it is the responsibility of the concerned parties to mutually agree upon a rearrangement schedule for specimens as part of the11 exposure program in order to minimize any effect that variations in irradiance might have as a function of specimen position. TEST METHOD A--CONTINUOUS EXPOSURE TO LIGHT AND INTERMITTENT EXPOSURE TO WATER SPRAY 6. Procedure 6.1 Apparatus shall be Type A, B, AH, BH, C, D, or E light-exposure device. 6.2 Program the instrument for continuous light and intermittent water spray in accordance with the manu facturer's instructions. Choice of the program.selected will be by mutual agreement among the interested parties. Histor- ; ical convention has established a cycle of 102 min of light 1 followed by a cycle of 18 min of light and water spray as a commonly accepted program that permits the attainment of the maximum black-panel temperature during the light-only portion of the cycle. 6.3 In Types AH and BH apparatus, adjust dry- and ! wet-bulb temperature controls, humidifier, and immersion ; heater controls to maintain the desired conditions as speci- ; fled in Section 5. In Types C, D, and E, adjust the chamber temperature and humidity controls to maintain desired j conditions as specified in Section 5. 6.4 In Types A and B with humidifier, humidity may be adjusted but not controlled. 6.4.1 Type B instruments without a humidifier musi operate with whatever humidity occurs from the evaporation of water in the bottom of the test chamber and from j specimen spray. TEST METHOD B--ALTERNATE EXPOSURE TO LIGHT AND 1 DARKNESS AND INTERMITTENT EXPOSURE TO WATER SPRAY 7. Procedure i 7.1 Apparatus shall be Type A, B, AH, BH, or E light'-tfj exposure device. , ! 7.1.1 Types AH, BH, and E apparatus with automatic ' humidity controls may be operated on alternate light and dark cycles. :j| 7.1.1.1 Operation during the light-on cycle shall be as described in Section 6. -- | 7.1.1.2 Separate controls for temperatures and humid-: ideation may be adjusted during the dark cycle for automatic control as the program alternates from light to dark. In Type BH and E apparatus, a rack spray to cool the specimens by J wetting the unexposed back surface can result in develop- ( ment of condensation on the exposed specimen surface j during the dark cycle. ; 7.1.2 Types A, B, AH, BH, and E may be programmed tb j operate on alternate light and dark cycles without control of ; relative humidity. TEST METHOD C--CONTINUOUS EXPOSURE TO LIGHT WITHOUT WATER SPRAY 1-1, radii 11 Reference Draft ISO Recommendation No. 177, Document ISO/TC-38 (Secretariat 102) 186. Scales with instructions for use are available from ISO member bodies in the various countries of the world. In the USA they may be obtained from The Secretary, American Association of Textile Giemists and Colorists, P.O. Box 12215, Research Triangle Park, NC 27709. 8. Procedure j 8.1 Apparatus shall be Types A, B, AH, BH, C, V, or f | light-exposure devices programmed for continuous light i only, in accordance with the manufacturer's instructions Optical filters C or D described in 4.1.2.1 should be used. * 1078 DU P050298256 # G 26 IW 3.1.1 Adjust the controls on the apparatus so that the apiaijS Ick-panel temperature is 63 + 3C (145 5F) and the gative humidity is 30 5 % when the xenon lamp is jerated at a wattage that provides 20 AATCC Fading Units iT ftexposure in about 15 to 25 clock hours. Check at regular lervals and, when necessary, readjust the controls to aintain the specified values for these variables. Target lues for black panel temperature, 20 AATCC Fading Sr HI pits, and relative humidity Should be 63"C, 20 clock hours, and | Id 30 %, respectively. anuH be l itor-j lil'ht J J' 5--20 AATCC Fading Units is equivalent to a 1.5 0.2 ilLAB(40) unit change in Blue Wool L-4 (#4 on the ISO Gray Scale), addition of about 110 kJ/m5 (1.5 W/ra2-20-h exposure) at 420 nm > been found suflicient to produce the specified condition. [8.1.2 Expose the material to be tested as determined by tt'df futual agreement among the concerned parties or, when not anly j lerwise specified, in accordance with one of the following: 18.1.2.1 yersus One AATCC Blue Wool Lightfastness and.; fandartP-Expox the test specimen and any mutually sion reed-upon AATCC Blue Wool Lightfastness Standard 'eci- itil the selected standard between its exposed and unex- iber psed portion exhibits a color change equal to Step 4 of the ired lO Gray Scale. Report the results by any mutually agreed- ton method of measuring change in the test specimen. d-bel : 8.1.2.2 Versus Set of AATCC Blue Wool Lightfastness tandards--Expose the test specimen and a set of AATCC mstS |lue Wool Lightfastness Standards until a maximum per ipfl missible amount of change, as determined by any specified om;| mutually agreed-upon method of measurement, occurs in ie test specimen. Assign it a classification njimber equal to rat of the numbered standard that most nearly exhibits a NO R tange in color equal to Step 4 on the ISO Gray Scale :tween its exposed and unexposed portion,: Where one Standard shows a color change greater than Step 4 and the text higher number standard shows less than a Step 4 color |hange, an intermediate or half-grade rating may be used. 8.1.2.3 Versus Other Standard Sample--Expose the test iticjg [Specimen and any mutually agreed-upon standard sample tnd jntii either, by any specified or mutually agreed-upon tethod of measurement, shows an agreed-upon amount of as inge. Report the results on the basis of a comparison of the specimen with the standard sample. TEST METHOD D--ALTERNATE EXPOSURE TO LIGHT AND DARKNESS WITHOUT WATER SPRAY 9. Procedure 9.1 Apparatus shall be Types A, B, AH, BH, or E programmed to predetermined cycles of light and darkness by turning off the xenon arc. N> ' 6--Type B instruments not equipped with a vaporizing unit do not meet the requirements of Test Method D. In Type A and Type B apparatus with intermittent blower operation during the light-off cycle and the atomizer in continuous operation, the test ehamber air temperature will drop to that of room air less the heat removed by vaporation of water from wicks and atomizer. 9.1.1 Unless otherwise specified, exposure conditions shall be identical to Test Method B except that during the light-on cycle the equilibrium condition for relative humidity shall be 35 5 % and during periods ofdarkness equilibrium conditions shall be%0 5% relative humidity at a dry-bulb temperature of 35 3C (95 5F). 10. Report 10.1 Report the following information: 10.1.1 Type and model of exposure device, 10.1.2 Type of light source and wattage, 10.1.3 Type and age of filters, 10.1.4 Spectral irradiance at sample location, W/m2-nm (see Note 9), 10.1.5 Irradiation, kJ/nj2, 10.1.6 Elapsed exposure time, h, 10.1.7 Light- or dark-water-humidity program employed, 10.1.8 Operating black-panel temperature, 10.1.9 Operating relative humidity, 10.1.10 Type of spray water, 10.1.11 Type of spray nozzle, and . 10.1.12 Specimen relocation procedure. No t ' 7--When direct measurement of'irradiation, and spectral irradiance cannot be made, data supplied by the manufacturer shall be substituted. Irradiation in kilojoules per square metre may be calculated by multiplying the product of the irradiance in watts per square metre and the exposure time in hours by the factor 3.6. lidttic j rpe ] by i sp ice to of ! E ;ht IS. 1079 DUP050298257 # G26 FJG. 4 Three-Tiered Specimen Rack The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard ere expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. .____ This standard Is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments wiii receive carefui consideration at a moating of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 1080 DUP050298258 h Designation: G 42 - 90 I Standard Test Method for Cathodic Disbonding of Pipeline Coatings Subjected to Elevated Temperatures1 Tills standard is issued under the fixed designation G 42; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (<) indicates an editorial change since the last revision or reapprovai. If Scope 11.1 This test method describes an accelerated procedure Sr determining comparative characteristics of insulating gating systems applied to steel pipe exterior for the purpose preventing or mitigating corrosion that may occur in hderground service where the pipe will be exposed to high Smperatures and is under cathodic protection. This test Jietfipd is intended for use with samples ofcoated pipe taken lom commercial production and is applicable to such pmples when the coating is characterized by function as an Electrical barrier. 1.2 This test method is intended for testing coatings Submerged or immersed in the test solution at elevated |mperature. When it is impractical to submerge or immerse he test specimen. Test Method G 95 may be considered vhere the test cell is cemented to the surface of the coated fipe specimen. If room temperatures are required, see Test lethod G 8. If a specific test method is required with no Options, see Test Method G 80. 1.3 The values stated in SI units to three significant Pecimals are to be regarded as the standard. 1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility ofthe |user of this standard to consult and establish appropriate `safety and health practices and determine the applicability of mregulalory limitations prior to use. jj (2. Referenced Document 2.1 ASTM Standards: G 8 Test Methods for Cathodic Disbonding of Pipeline 'Coatings2 G 12 Test Method for Nondestructive Measurement of Film Thickness of Pipeline Coatings on Steel2 G80 Test Method for Specific Cathodic Disbonding of Pipeline Coatings3 G95 Test Method for Cathodic Disbondment Test of Pipeline Coatings (Attached Cell Method)3 i 3. Summary of Test Method 3.1 This test method subjects the coating on the test I specimen to electrical stress in a highly conductive electroI lyte. The coating is artificially perforated before starting the 1 This method is under the jurisdiction of ASTM Committee GO on Durability of Nonmetallic Materials and is the direct responsibility of Subcommittee G03.O6 on Durability of Pipeline Coatings and Linings. Current edition approved May 25, 1990. Published July 1990. Originally published as G 42 - 75T. Last previous edition G 42 - 35. 2 Annua! Bool< ofASTM Standards, Vols 06.01 and 14.02. ' Annual Book ofASTM Standards, Vo! 14.02. test. The electrical stress is produced by connecting the test specimen to the negative terminal of a source of direct current and by connecting an anode to the positive terminal. Electrical instrumentation is provided for measuring the current flowing in the cell. The electrical potential is also measured and the specimen is physically examined at intervals during the test period and upon conclusion of the test. 3.1.1 The cathodic stress is applied under conditions of a constant-elevated temperature. 4. Significance and Use 4.1 Damage to pipe coating is almost unavoidable during transportation and construction. Breaks or holidays in pipe coatings may expose the pipe to possible corrosion since, after a pipe has been installed underground, the surrounding earth wil be moisture-bearing and will constitute an effective electrolyte. Applied cathodic protection potentials may cause loosening of the coating, beginning at holiday edges. Sponta neous holidays may also be caused by such potentials. This test method provides accelerated conditions for cathodic disbondment to occur and provides a measure of resistance of coatings to this type of action. 4.2 The effects of the test are to be evaluated by physical examinations and monitoring the current drawn by the test specimen. Usually there is no correlation between the two methods of evaluation, but both methods are significant. Physical examination consists of assessing the effective contact of the coating with the metal surface in terms of observed differences in the relative adhesive bond., It is usually found that the cathodically disbonded .area propa gates from an area where adhesion is zero to an area where adhesion reaches the original level. An intermediate zone of decreased adhesion may also be present. 4.3 Assumptions associated with test results include: 4.3.1 Maximum adhesion, or bond, is found in the coating that was not immersed in the test liquid, and 4.3.2 Decreased adhesion in the immersed test area is the result of cathodic disbondment. 4.4 Ability to resist disbondment is a desired quality on a comparative basis, but disbondment in this test method is not necessarily an adverse indication of coating performance. The virtue of this test method is that all dielectric-type coatings now in common use will disbond to some degree, thus providing a means of comparing one coating to another. 4.5 The current density appearing in this test method is much greater than that usually required for cathodic protec tion in natural environments. 4.6 That any relatively lesser bonded area was caused by electrical stressing in combination with the elevated and or 1081 DU PO50298259 G 42 depressed temperature and was not attributable to an anomaly in the application process. Ability to resist disbondment is a desired quality on a comparative basis, but most insulating materials will disbond to some extent under the accelerated conditions of this test. Bond strength is more important for proper functioning of some coatings than others and the same measured disbondment for two different coating systems may not represent equivalent loss of corro sion protection. 4.6.1 The amount of current flowing in the test cell is a relative indicator of the extent of areas requiring protection against corrosion; however, the current density appearing in this test is much greater than that usually required for cathodic protection in natural, inland soil environments. 4.6.2 Test voltages higher than those recommended may result in the formation of chlorine gas. The subsequent chemical effects on the coating could cast doubt on the interpretation of the test results. 5.Apparatus 5.1 Test Vessel--A suitable nonreactive vessel shall be used, capable of withstanding internal heating at not less than 60C and suitable for continuous circulation of the electrolyte. A 19-L (5-gai) cylindrical glass vessel has been found suitable, having an approximate diameter of 300 mm (12 in.) and a depth of 300 mm. A flat bottom is required for operation of a magnetic stirring rod. Dimensions of the vessel shall permit the following requirements: 5.1.1 Test specimens shall be suspended vertically in the vessel with at least 25 mm (1 in.) clearance, from the bottom. 5.1.2 Test specimens shall be separated by not less than 38 mm (1 lh in.), and a vertically suspended anode can be placed at an equal distance from each specimen not less than the separation distance. 5.1.3 Test specimens shall be separated from any wall of the vessel by not less than 13 mm (`A in.). 5.1.4 Depth of electrolyte shall permit the test length of the specimen to be immersed as required in 7.4. 5.1.5 The reference electrode may be placed anywhere in the vessel, provided it is separated from the specimen and from the anode by not less than 38 mm (11h in.}. 5.2 Anode--The anode shall be provided with a factory' sealed, insulated copper wire lead.4 5.3 Connectors--Wiring from anode to test specimen shall be 4107 cmil (14-gage Awg), minimum, insulated copper. Attachment to the test specimen shall be by sol dering or brazing to the nonimmersed end, and the place of attachment shall be coated with an insulating material. A junction in the connecting wire is permitted, provided that it is made by means of a bolted pair of terminal lugs soldered or mechanically crimped to clean wire ends. 5.4 Holiday Tools--Holidays shall be made with conven tional drills of the required diameter. For use in preparing small-diameter pipe specimens such as 19-mm (%-in.) nom inal diameter pipe, the use of a drill modified by substantially grinding away the sharp cone point has been found effective in preventing perforation of the metal wall of the pipe. A 4 Duriryn. a material found suitable for this purpose is available from Duriron Co., Inc.. Dayton. OH. sharp-pointed knife with a safe handle is required for use in making physical examinations. 5.5 Multimeters: 5.5.2 Multimeter, for direct current, having an internal resistance of not less than 10 Mft and having a range from 0.01 to 5 V for measuring potential to the reference electrode. 5.5.2 Multimeter, for direct current, having an internal resistance of not less than 11 MO and capable of measuring as low as 20 pV potential drop across a shunt in the test cell circuit 5.5.3 Multimeter, for initial testing of apparent coating resistance. 5.6 Reference Electrode--Saturated Cu CuS04 elkttrode having a potential of -0.316 V with respect to-the standardhydrogen electrode shall be the standard of reference in these1: test methods. Other electrodes may be used but measure-* meats thus obtained shall be converted to the Cu CuS04 reference for reporting by making the proper correction. " N' I--A saturated Cu CuSO, electrode reading --1.50 V at 25"C will read -1.53 V at 60"C, a scale increase of 0.03 V. 5.6.1 A saturated calomel electrode at 25C is converted to Cu CuSO,, by adding -0.07 V to the observed reading. If . the saturated calomel electrode reads -1.43 V at 25C, it will read -1.46 V at 60C, a scale increase of 0.03 V, It follows that a saturated calomel electrode reading of--1.46 V at 60C is equal to a saturated Cu CuS04 reading of--1.50 V at 25"C. 5.6.2 A 0.1 normal calomel electrode at 254C is converted * to Cu CuS04 by subtracting -0.02 V from the observed reading. Since the potential change due to an increase from 25 "C to 60C is negligible, it follows that a 0.1 normal calomel electrode reading --1.52 V at 60C is equal to a saturated Cu CuS04 reading of -1.50 V at 25C. 5.7 Thermometers, two, mercury-filled type, accurate to \ 1 "C. One shall be of the fuLI-immersion type for measuring temperature near the bottom of the vessel, and a second j thermometer shall be of the partial-immersion type for ; measuring temperature near the top-of the vessel. 5.8 Combination Heater Plate, with built-in magnetic j stirrer, or equivalent, shall be used for heating and stirring the electrolyte. The heater shall be adjustable to produce and control a temperature of 60 1C in the test vessel. 5.9 Direct-Current Rectifier, capable of supplying con stant current at a voltage of 1.50 0.01 V, as measured between the specimen and reference cell. 5.10 Thickness Gage, for measuring coating thickness in accordance with Test Method G 12. 5.11 Precision Resistor, lft 1 %, 1 W (min), to be used in the test cell circuit as a shunt for current. 5.12 Carbon or Stainless Steel Electrode, used temporarily. with the volt-ohm-meter to determine apparent initial hol iday status of the test specimen. 5.13 Additional Connecting Wires, 4107 cmil (14-gage Awg), minimum, insulated copper. 5.14 Brass Studs, used at a terminal board, together with alligator clips or knife switches, for making and breaking circuits. Alligator clips shall not be used to connect the electrodes or specimens at the top location of test cells. 6. Reagents and Materials 6.1 The electrolyte shall consist of potable tap water or ; NOI a.) in;. Iqrforaf |f perf* itandai! i'subsif ' . Nora 7.3 1082 DU PO50298260 'gher purity water (distilled or demineralized water is tisfactory) with the addition of 1 weight % of each of the (lowing technical-grade salts, calculated on an anhydrous asis: sodium chloride, sodium sulfate, and sodium car inate. (N' 2--The resulting solution has a pH of 10 or higher and a sistivity of 25 to 50 SI cm at room temperature. } 6.2 Materials for sealing the ends of coated pipe, speci mens may consist of bituminous products, wax, epoxy, or (her materials, including molded elastomeric or plastic end tips, capable of withstanding the test temperature. 6.3 Plywood has been found suitable for the construction T nonconductive test vessel covers and for the support rough apertures of test specimens and electrodes. Wood owefs introduced through holes in the top ends of test `ecimens have been found suitable for suspending test `pecimens from the vessel cover. . Test Specimen 7.1 The test specimen shall be a representative piece of jjroduction-coated pipe. One end shall be plugged, sealed, or capped. 7.2 One holiday shall be made, in the middle of the immersed length by drilling a radial hole through the coating o that the angular cone point of the drill will fully enter the Steel where the cylindrical portion of the drill meets the steel surface. The drill diameter shall be not less than three times the coating thickness, but it shall never be less than 6 mm. (% in.) in diameter. The steel wall of the pipe shall not tie perforated. With small-diameter pipes, where there is danger of perforating the pipe, the holiday shall be started with a standard,60" cone point and finished with a drill that has had a substantial portion of the cone point ground away. No t ' 3--Before making the holiday, see 7.5. 7.3 The end of the pipe which will protrude above the immersion line shall be provided with suitable supporting means and a separate wire connection for electrical purposes, soldered, or brazed to the pipe. The protruding end, in cluding hanger and wire connections, shall be protected and sealed with an insulating coating material. 7.4 The specimen test area shall consist of the area between the edge of the bottom end seal and the immersion line. The bottom end seal area shall not be considered part of the area tested. Coated specimens of any suitable diameter and length of pipe may be used, but the immersed area shall be not less than 23 200 mm2 (36 in.2). An area of 92 900 mm2 (1 ft2) has been found preferable when convenient. 7.5 The continuity ofthe coating and efficiency.ofthe end seal, shall be tested before making artificial holidays as follows: 7.5.1 Immerse the test specimen and a carbon or stainless steel electrode in the electrolyte. Connect one terminal of the ohmmeter to the test specimen and the other terminal to the carbon or stainless steel electrode. Measure the apparent resistance in ohms, making two determinations: one with the specimen connected to the positive terminal of the ohmmeter, and one with the specimen connected to the negative terminal. The lowest of the two readings should be not less than 1000 Mfi, however, the test may be conducted with a low reading less than 1000 MS2, provided that the condition is taken into account in evaluating results. 8. Procedure 8.1 Immerse the test specimen in the electrolyte and connect it to the anode as shown in Fig. 1. Adjust the rectifier-.or voltage divider so that the potential between specimen and reference cell is -1.50 0.01 V at 25C (-1.53 0.01 V at 60C) (see Fig. 2). Position the holiday to face toward the anode. Space the anode with respect to test specimens as required in 5.1. Mark, the correct immersion level on the exterior of the test vessel and maintain by daily N' --For multiple specimens in the same test vessel, see Fig. 2, for circuit diagram using voltage dividers. FIG. 1 Test Set-Up for Cathodic Disbonding Test at Elevated Temperature 1083 DU P 050298261 # G 42 Sei reclifEer output voltage to not over 3voltsihen trim eoch voltage divider so that A to C measures 1.5 volts. IOO OHM, 25 WATT RHEOSTATS VOLTAGE DIVIDERS} fily ur Jble d iter sc ft-6'2 |idenct ge of 8.6.3 ffs noi l the |tlow f8.6.4! {tempt a si- ftersec Isistan Inside: Bating jfi'8.6.55 amers oint o: To measure current use terminals A and 8 To measure voltage use terminals A and C ^-REFERENCE CELL FIG. 2 Circuit Diagram for Cathodic Disbonding Test additions of preheated, distilled, or demineralized water as required. 8.2 The temperature of the electolyte surface to bottom shall be not less than 60 3'C. The electrolyte shall be continuously circulated by means of the stirring apparatus or equivalent. The maximum temperature shall be attained 4 1 h after starting the heater and immersing the specimen. N' 4--Throughout the test period, ejected sealant or salt deposits, or both, may form near, or partially obstruct the intentional coating holiday described in 7.2. No attempt shall be made to dear ihe holiday while the test is in progress. 8.3. Electrical Monitoring Schedule: 8.3.1 Electrical measurements shall be made on the start up day and on each normal working day thereafter for the duration of the test. A maximum of three consecutive nonworking days shall be preceded by at least two working days; one non-working day or two consecutive non-working days shall be preceded by at least one working day, except at start-up and termination when three and two working days are required, respectively. 8.3.2 Electrical measurements characterizing the start of the test are defined as the average of measurements taken on the second and third days after immersion. 8.3.3 Electrical measurements characterizing intermediate and terminal time spans shall be taken on two successive days prior to and including the target date. 8.4 Electrical measurements and adjustments made each normal working day: 8.4.1 Measure E2, the stress potential in volts between the test specimen and the reference electrode, without discon necting the energized anode or specimen from the circuit. Use the high-resistance voltmeter described in 5.5. The stres-, potential, Ely should measure -1.50 0.01 V at 25"C (-L53 0.01 V at 60C); if it does not, adjust the rectifier or voltage divider accordingly. 8.4.2 After Ez has been measured and adjusted, if neces sary, measure /,, the current demand in amperes, by determining the potential drop across the l-.Q precision resistor permanently installed in the test cell circuit with the high-resistance voltmeter described`in 5.2. The voltage reading will be numerically equal to amperes. N' 5--An alternative method of measuring current _deman_ utilizes a zero-resistance ammeter. In this method, the wire connection between the test specimen and~anode is temporarily broken and a zero-resistance ammeter temporarily interposed between the specimen and the anode. Reconnect the specimen to the anode with the connector wire as soon as this measurement is completed. 8.4.3 Measure j, the polarized potential, in volts, usiry the high-resistance voltmeter described in 5.5 connected between the test specimen and the reference electrode it1 follows: 8.4.3.1 Disconnect the anode from the test specimen while closely observing the high-resistance voltmeter. As the instrument pointer falls, it will dwell significantly at the polarized potential before recording further. The dwell point is j. 8.5 Standard duration of the test period shall, be 30 days (720 h) in the energized test vessel including warm-up and cool-down times, unless longer test periods are specified. 8.6 A physical examination shall be performed immedi ately upon termination of the test period as follows: 8.6.1 Before examination, wash the test specimen care- 1084 ; i. ' i:i DU P050298262 # G 42 der gently flowing tap water without disturbing estructive effects. Adjust the temperature of the tap that it approximates that of the room temperature. Examine the entire immersed area visually for any of new holidays and loosening of coating at the all holidays, including the artificial holiday. Drill a new test hole in the coating in an area that immersed, staying away from the immersion line Scut end. Recommended distances are given in Fig. 3. the same drilling procedure described in 7.2. ! In order to gage or calibrate the lifting technique, to lift the coating at the new test hole with the point arp knife after, making cuts through the coating ting at the center of the hole. Inability or relative ce to lifting or disbonding the coating shall be red the adhered or bonded condition of the untested with respect to the lifting technique used. Determine if the coating has been loosened at the sedjest hole by attempting to lift the coating with the f a'sharp knife after making cuts through, the coating intersecting at the holiday or point of inspection using the same technique applied in 8.6.4. Classify coating that can be lifted or disbonded more readily than at the new test hole as unsealed area. Measure the unsealed area. N' 6--The use of a transparent film having a grid laid out in small squares such as 2.54 mm (0.1 in.) on a side has been found useful. The film is placed against the unsealed area and the boundary ofthe unsealed area is traced on the grid. The area is then obtained by counting the squares within the bounded area. 8.7 Determine and record the resistivity and pH of the electrolyte at the beginning and end of the test period. 9. Report 9.1, The report shall include the following (see Fig. 4): 9.1.1 Complete identification of the test specimen, in cluding: 9.1 i 1.1 Name and code number of the coating, 9.1.1.2 She of pipe, DIMENSION A' e c D E ' -F MILLIMETRES 490.22 12.7 245.11 12.7 114.3 6.35 233.363 MIN 19.05 MIN 762 MIN INCHES (19.300 0.500) (9.650 0.500) (4,500 0.250) (9.1875, min) (0.750, min) (30, min) FIG. 3 Recommended Dimensions for Specimen 1085 DUPO 502 98263 Cathodic Disbonding of Pipeline Coatings Subjected to Elevated Temperatures Specimen . Production Date_____________________ Coating-------------------------------__----- Production Run No.. Applied by . Thickness, mm (in.}: Max - Min. Date Started---------------- pH @ 25C_ Date Finished- pH @ 25C_ Immersed Area, mm2 (in.8) . Holiday Diameter, mm (in.) . Date Elapsed Days Temperature, C Electrolyte Hi. V # G 42 DATA SHEET AND REPORT Target, C Electrolyte _ At Holiday (1). Ohm-cm @ 25C . Ohm-cm @ 25C. -Initial Ohms: + __ (2)- Report j Initials i <3)_ (.'2 The! ibefora, t ,{ kal dat f&u&re fdianU Th .4cal r *4.1 (, cteris ' 2,v Average Valdes on | AE Target Days . | (lA V AE. V 'i.(tA HT J cr ------ ------- .-ffl iI . -illlll iS ` fei -| i Physical Examination at Termination: Area Disbonded Less Initial Holiday Total Unsealed Area (net) * Equivalent Circle Diameter. Change: Start to Termination: mm2 (in.2) Circ. Da mm (In.) FIG. 4 Suggested Form for Use in Presenting Data I _______ J Comments: 9.1.!.3 Source, production date, and production run number, 9.1.1.4 Minimum-maximum coating thickness, 9.1.1.5 Immersed area, 9.1.1.6 Size and number of initial holidays, and 9.1.1.7 Dates of starting and terminating test. 1086 DUP050298264 G 42 9.1.2 The relative resistances of the test specimen, in Ohms, before the artificial holiday was made as described in ?.5. 9.1.3 Tally of areas that have been found unsealed on the ![terminal date. Areas may be reported in square millimetres lor square inches) or millimetres (or inphes) of equivalent 'circle diameter of the area, or both. 9.1.4 The results of starting, intermediate, and terminal lelectrical measurements. Report the following measure- Imetits: 9.1.4.1 Current demand in microamperes or negative jjpharacteristic of the logarithm of the current in amperes, in [both, 9.1.4.2 The value of AE = E2~ E;, in volts, and 9.1.4.3 Change from start to termination for values in |9.1.4.1 and 9.I.4.2. 9.1.5 Temperature of the electrolyte at approximately the |same hour each working day. 9.1.6 Other information that may be pertinent. 10. Precision and Bias 10.1 Precision data are limited to two adjacent specimens I taken from the same production-coated pipe and assumed I that the production process was uniform wilii respect to pipe surface condition and coating material. Specimens that were not adjacent in the as-produced condition or were taken from different lengths of pipe may represent differing process conditions. The following data should be used forjudging the acceptability of results. (These precision data are approxima tions based on limited data, but they provide a reasonable basis forjudging the significance of results.) 10.2 Repeatability--Duplicate results obtained within a laboratory should be acceptable unless they differ by more than 25 mm (1 in.) in value D in accordance with the following equation: D = (A/a.lS5)Vt where: A =unsealed area developed from one artificial holiday, mm2 (or in.2) or if they differ by more than unity in the negative characteristic of the logarithm of the current demand in amperes. 10.3 Reproducibility--The results reported by one labora tory should be acceptable unless they differ from those of another laboratory by more than 25 mm (1 in.) for the value D in the equation given in 10.2, and by more than unity in the negative characteristic of the logarithm of the current demand in amperes. The American Society for Testing and Materials takes no position respecting the validity ofany patentrights asserted in connection with any item mentioned In this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standardis subject to revision at any time by the responsible technical committee and mustbe reviewedevery five years and ifnot revised, either reapproved or withdrawn. Your continents are invitedeither for revisionofthisstandard orforadditional standards and should be addressed to ASTM Headquarters. Your comments wifi receive careful consideration at a meeting of the responsible technical committee, which you may attend, ft you feef that your comments have hiot received a fair hearing you should 'make your views known to the A$TM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. DUP0502 98265 Designation: G 53 - 88 Standard Practice for Operating Light- and Water-Exposure Apparatus (Fluorescent UV-Gondensation Type) for Exposure of Nonmetallic 1 ' Materials1 This standard is issued under the fixed designation G 53; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the,yearoflast revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon {) indicates an editorial charige since the last revision or reapproval. 77?/.? standard has been approved for use by agencies ofthe Department ofDefense. Consult the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department.of Defense. 1. Scope 1.1 This practice covers the basic principles and operating procedures fot using fluorescent ultraviolet (UV) and con densation apparatus to simulate the deterioration caused by sunlight and water as rain or dew. 1.2 This practice is limited to the method of obtaining, measuring, and controlling the conditions and procedures of exposure. It does not specify the exposure conditions best suited'for the material to be tested. Specimen preparation, and evaluation of the results are covered in ASTM test methods or specifications for specific materials. 1.3 The values stated in SI units are to be regarded as the standard. 1.4 This standard may involve hazardous materials, oper ations, and equipment. This standard does noUpurport to address all ofthe';safety problerhs associated with its Use. It Is; the responsibility of'the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: E 220 Method for Calibration of Thermocouples by Com parison Techniques2 G7 Practice for Atmospheric Environmental Exposure Testing of Nonmetallic Materials3 2.2 CIE Standard: . No. 20 Recommendations for the Integrated Irradiance and the Spectral Distribution of Simulated Solar Radia tion for Testing Purposes4 3. Description of Terms Specific to This Standard 3.1 irradiance--the radiation incident on a surface ex pressed in W/m2. Irradiance is the total of the incident radiation at all wavelengths. Forty watt fluorescent lamps of the UV-B and UV-A types generate similar amounts of irradiance. However, since this irradiance is distributed, at, different wavelengths, the photochemical, effects caused by these different lamps vary greatly. Therefore, irradiance should not be used,to- compare DY light sources,::. 3.2 spectral irradiance--distribution of irradiance as a function of wavelength. It is expressed in W/m2 per wave length band. The spectral irradiance of sunlight is often sfrowii as'W/m2 per 10 nm band; The spectral irradiance of fluorescent UV |amps should be shown in b^nds 1 or 2 nni. wide. Spectral irradiance is the proper method for comparing' sources with different energy distributions. 3.3 spectral energy distribution-(SED)--general term for the characterization of the amount of radiation present at each wavelength. SEDs can be expressed by power in watts, irradiance in W/m2, or energy in joules. Tjie shape of the SED. would be identical in all of these units. Fluorescent lamps are frequently described by relative SEDs which show the amount of radiation at each wavelength as a percentage ofthe amount of radiation at the peak wavelength. Fig. 1 is a relative SED. 3.4 ultraviolet regions--CIE Publication No. 20 (1972) divides the ultraviolet spectrum into three regions: UV-A, radiation in wavelengths between 315 nm and 400 nm; UV-B, radiation in wavelengths between 280 nm and 315 nm; and UV-C, radiation in wavelengths shorter than 280 nm. 3.5 fluorescent UV lamp-lamp in which radiation at 254 nm from a low-pressure mercury arc is transformed to longer wavelength UV by a phosphor. The spectral energy distribu tion of a fluorescent UV lamp is determined by the emission 1 This practice is under the jurisdiction of ASTM Committee G-3 on Durability of Nonmetallic Materials, and is the direct responsibility of Subcommittee G03.03 on Simulated and Controlled Environmental Tests. Current edition approved July 29,1988. Published September 1988. Originally published as G 53 - 77. Last previous edition G 53 - 84. 2 Annual Book ofASTM Standards. Vol 14.03. 3 Annual Book ofASTM Standards. Vol 14.02. 4 Available from Secretary, U.S. National Committee, CIE, National Bureau of Standards. Gaithersburg, MI> 20899. 1088 'V-: sf;:.. DUP050298266 ictrum of the phosphor and the UV transmission of the Ss tube. |Sammary of Practice p.l Specimens are alternately exposed to ultraviolet light e and to condensation alone in a repetitive cycle. %2 The UV source is an array of fluorescent lamps, with p emission concentrated in the UV range. 4.3 Condensation is produced by exposing the test surface ?a heated, saturated mixture of air and water vapor, while fe reverse side of the test specimen is exposed to the cooling fluence of ambient room air. 4.4 The exposure condition may be varied by selection of: e fluorescent UV lamp; the timing of the UV and ndensation exposure; the temperature of UV exposure; d the temperature of condensation exposure. Significance and Use 5.1 The use of the apparatus under this practice is tended to simulate the deterioration caused by water as 'n or dew and the ultraviolet energy in sunlight. It is not tended to simulate the deterioration caused by localized eather phenomena, such as atmospheric pollution, biologcal attack, and salt water exposure, i 5.2 Variation in results may be expected when operating "nditions are varied within the accepted limits of this ractice. Therefore, no reference shall be made to results rom use of this practice unless accompanied by a report "etailing the specific operating conditions in conformance :th Section 11. 5.3 Any report correlating results from use ofthis practice i results from a period of natural weathering shall specify in detail the conditions of natural exposure, since sunlight and jwater effects upon materials exposed to the weather will vary from year to year and also vary with location, latitude, time of year, temperature, proximity to water sources, etc. N' 1--Practice G 7 lists the information required to describe a particular condition of outdoor exposure. 5.4 Correlations established and reported in conformance with 5.2 and 5.3 shall not be extrapolated to other test conditions permitted by this practice, to other conditions of natural exposure, or to materials other than those tested. 6. Apparatus5 6.1 Test Chamber, (see Fig. 2) constructed of corrosionresistant materials enclosing eight fluorescent UV lamps, a heated water pan, test specimen racks, and provisions for controlling and indicating operating times and temperatures. 6.2 Lamps, rapid start, medium bipin fluorescent UV lamps with a length of 1220 mm, and a nominal rating of 40 W when operated from a ballast providing a controlled current of 430 mA at 102V. 6.2.1 Unless otherwise specified, the lamps shall be UV-B lamps with a peak emission at 313 nm and a spectral energy distribution as shown in Fig. 1. 6.2.2 Other fluorescent UV lamps meeting the size and electrical characteristics in 6.2 may be used, provided that the lamp and spectraf energy' distribution are reported in conformance with Section 11. 6.3 Lamp Spacing and Arrangement--The lamps shall be mounted in two banks of four lamps each as shown in Fig. 2. The lamps in each bank shall be mounted parallel in a flat plane on 70-mm centers. 6.4 Specimen Mounting and Arrangement--The test spec imens shall be mounted in stationary racks with the plane of the test surface parallel to the plane ofthe lamps at a distance of 50 mm from the nearest surface ofthe lamps, as shown in Fig. 2. 6.4.1 The test specimens shall be exposed within an area 210 mm in height by 900 mm wide on each side of the apparatus located as shown in Fig. 4. N' 2--It is possible to mount specimens above, below, and beside the 210 by 900 mm area, but specimens so mounted will be exposed to lower UV intensities. 6.5 Condensation Mechanism--Water vapor shall be gen erated by heating a water pan extending under the entire sample area and containing a minimum water depth of 25 mm. Specimen racks and the test specimens themselves shall constitute the side walls of the chamber. The back side of the LAMP ROTATION 5 Apparatus and lamps from Q-Panel Co., 26200 First St., Cleveland, OH 44145, and from Atlas Eieotric Devices Co., 4114 N. Kavenswood Ave., Chicago, IL 60613, have been found satisfactory. DUP0502 98267 G 53 a ol naif uniform UV mnily ...........- "V, - 'tiirtJ---- . FIG. 4 Limits of Area of Uniform Intensity specimens shall be exposed to cooling effects of ambient room air. The resulting heat transfer causes water to con dense on the test surface. 6.5.1 The specimens shall be arranged so that condensate runs off the test surface by gravity and is replaced by fresh condensate in a continuous process. Vents along the bottom of the test chamber shall be provided to permit an exchange of ambient air and water vapor to prevent oxygen depletion of the condensate. 6.6 Water Supply, with an automatic control to regulate the level in the water pan shall be provided. Distilled, deionized, or potable tap water are equally acceptable for purpose? of the test, since the condensation process itself distills water onto the test surface. 6.7 Cycle Timer, a continuously operating cycle time, for programming the selected cycle of UV periods and conden sation periods. 6.7.1 Hour meters shall be provided to record total time of operation and total time of UV exposure. 6.8 Specimen Temperature Measurement: 6.8.1 Specimen temperature shall be.measured by a ther mometer with a remote sensor attached to a black aluminum panel 75 by 100 by 2.5 mm thick. The thermometer shall be precise to 1C through a range from 30 to 80C. The indicator dial shall be located outside the test chamber. 6.8.2 The black aluminum panel with the thermometer sensor shall be positioned in the center of the exposure area so that the sensor is subject to the same conditions as the specimens. 6.9 Specimen Temperature Control: 6.9.1 During UV exposure, the selected equilibrium tem perature shall be maintained within 3C by supplying heated air to the test chamber. 6.9.2 During condensation exposure, the selected equilib rium temperature shall be maintained within 3C by heating the water in the water pan. 6.9.3 The UV and condensation temperature controls shall be independent of each other. 6.9.4 Doors shall be located on the room air side of the specimen racks to act as insulation during the UV exposure and to minimize drafts. Such doors shall not interfere with the room air cooling of the specimen during the condensa tion exposure. 6.10 Test Chamber Location: 6.10.1 The apparatus shall be located in an area main tained at a temperature between 20C and 30C. The room temperature shall be measured by thermometers mounted on interior walls or column approximately 1500 mm above the floor level and at least 300 mm from any heated apparatus, Three or more thermometers located at various points will show any temperature variation in the area. 6.10.2 It is recommended that the apparatus be located at least 300 mm from walls or other apparatus. Nearby heat sources, such as ovens or heated test apparatus, should be avoided or shielded, because such heat sources can reduce the cooling required for condensation. 6.10.3 The room where the apparatus is located, shall be ventilated to remove, the heat and moisture produced and to maintain the temperatures specified in 6.10.1. Two to four a;r rhaticpc rif*r P< ' * wifi nnrmallv rvr/AxriHA _. 7. Test Specimens .7,1 Replicate specimens are desirable to provide a record, of degradation at different tiipe intervals. Retention of an unexposed specimen is recommended as it is difficult to. mask a specimen to prevent exposure to .condensation. 7.2 For specimens of insulating materials, ,such a^.wood; plastic, m porous laminates, maximum specimen thickness should be 20 mm to allow adequate heat transfer, fpr condensation. 7.3 To provide rigidity, flexible specimens may be at tached to a backing panel made of aluminum or other noncorrosive heat conductive material. 7.4 Gut edges of coated steel specimens shall be protected so that bust does not contaminate the test surface. 7.5 Holes in specimens and any openings larger than 1 mm around irregularly shaped specimens shall be sealed to prevent loss of water vapor. Porous specimens, such as textiles or wood shall be backed with a vapor barrier such as metal or plastic.' 8. Calibration and Standardization 8.1 The thermometer or thermocouple which indicate? test temperature shall be calibrated by immersing the sensing element and a liquid-in-glass thermometer in water heated to approximately 70C and cofnparing the two temperatures as in Method E220. ' '' 8.2 The formation of'condeilsation may be observed by using clear glass or plastic blanks in the specimen holders or rack. One large sheet of plastic may also be' used for this purpose. The condensate that forms on a ,given area during a period of condensation may be collected and then, measured. 8.3 The fading and other changes caused by the fluores cent UV lamps may be observed by exposing li'ghtfastneSS standards in'the apparatus using UV alone without conden sation. ' 8.3.1 The AATCC Blue'Wool Lightfastness reference materials6 may be used to measure the changes caused by UV. The L2 Blue Wool has been found satisfactory for evaluating fluorescent UV lamps. , 8,3.2 Other lightfastness reference -materials may be used by agreement. 8.4 Reference standards for calibrating the operation of the apparatus in alternate exposure to UV light and conden sation may be prepared from painted metal, plastics, or other materials. Painted metal specimens produced by the coil- coating process have been found suitable for such reference standards. 9. Procedure 9.1 Mount the test specimens in the specimen racks with e Available from American Association of Textile Chemists and Colorists, P.O. Box 12215, Research Triangle Park, NC 27709. 1090 9.3.|; Rite liii .jtmp4 |ondd 9.3U G COt period, leach!.' 9.3.1 ienvifop. 9.3.f affectej limctt increa^ expose densati while 4 Ion wot > is DUP050298268 G 53 test surfaces facing the lamp. When the test specimens do completely fill the racks, fill the empty spaces with blank iels to maintain the test conditions within the chamber. p.2 Program the selected test conditions. Operate contin|usly, repeating the cycle, except for servicing the instru ct and inspection of specimens. t3 Various test conditions may be used. If no conditions jp specified, the following cycle and temperatures are Sgested: 4 h UV at 60C, 4 h Condensation at 50C. |N' 3--Prior versions of this practice recommended a condensa- |n temperature of 40'C in 9.3. When operating in room conditions |at do not comply with those set forth in 6.10, a 40"C condensation iperature can result in inadequate condensation. Therefore, a 50"C |ndensation temperature is now suggested. 9.3.1 Any test temperature that can be maintained within ie limits specified in 6.9.1 and 6.9.2 may be used. UV test iperature of 50C, 60C, and 70C are widely used. A fjbndensation test temperature of 50C is commonly used. 9.3.2 The Following time cycles are widely used: 4 h UV/4 CON, and"8 h UV/4 hr CON. Use UV and condensation leriods of at least 2-h duration to allow sufficient time to :ach equilibrium. 9.3.3 The severity of the UV exposure is influenced by test imperatures and time cycles. Photochemical reaction begins is soon as the UV lamps are turned on. The rate of UV degradation is proportional to the time of UV exposure or ie temperature of UV exposure, or both. UV exposures at jemperatures higher than those expected in the service mvironment can cause abnormal thermal degradation. 9.3.4 Water reactions during condensation exposure are iffected by the permeability of the specimen and require time to initiate.The rate of water degradation is increased by increased temperature. However, long hot condensation ixposures can cause abnormal degradation. Four-hour conlensation exposures are often used for paints on metals, hile condensation exposures of 20 h duration may be used [on wood. 9.4 Maintenance--Periodic maintenance is required to maintain uniform UV and condensation exposure condi tions. 9.4.1 After 400 to 450 h of lamp operating time, replace one lamp in each bank of lamps, and rotate the other lamps as shown in Fig. 3. This procedure provides a useful lamp life of 1600 to 1800 h. 9.4.2 Drain water and clean water pan when conducting lamp replacement and rotation procedure. Scum on the top of the water can inhibit water vaporization. 9.5 Sample Rotation--The samples' positions within the test area should be rotated on a regular basis in order to minimize any effects from horizontal or vertical variations in UV or temperature. The sample rotation sequence should provide that all samples spend approximately the same amount of exposure time near the center of the exposure area and near the edges of the exposure area. The following rotation sequence is recommended: 9.5.1 Horizontal Rotation--Once a day rotate the ex treme left hand and extreme right hand samples into the center as shown in Fig. 6. 9.5.2 Vertical Rotation--Rotate the samples vertically so that each sample spends the same amount of exposure time in each vertical position in the sample holder. For instance, if two samples are stacked vertically in each sample holder, then the top and bottom sample should switch places halfway through the test method. If four samples are stacked vertically, then the samples should be repositioned vertically three times during the test method. 9.5.3 Other sample rotation sequences may be used by agreement. 9.6 Inspect specimens daily in tests with a length of 1 week or less. Tests for longer periods should be inspected weekly. 9.6.1 A permanent record of degradation at various times may be obtained by using three replicate specimens and REPORT FORM TEST No.:_____ ASTM PRACTICE G- 53 APPARATUS Type and Model MANUFACTURER, TYPE SPECIAL TEST CONDITIONS _C. / FLUORESCENT-UV I CONDENSATION TEST ----------------- By:---------------------------------------- TEST TIME. PEAK EMISSION nm. LOW CUTOFF (IK cl peck) _________ nm START DATE: END DATE: SPECIMEN SIZE. MATERIAL PROPERTIES TO BE MEASURED !. __________________ TIMER H'fcS. START TIMER HRS. STOP j Rotated LAMP SERVICE at hr*. D Yes DNo MEASURING PROCEDURE (ASTM Spec., atc.l FIG. 5 Sample Report Form 1091 DU P0502 98269 G 53 removing the replicates sequentially at intervals equal to one third of the test length. 9.7 Conclude the test when either a mutually agreed-upon number of total test hours or a mutually agreed-upon change has occurred in the test specimen or a standard test spec imen. For convenience in inspecting and concluding tests during normal working hours, the following test durations are recommended: 96 h -- 4 days 168 h = 1 week 336 h = 2 weeks 504 h = .3 weeks 672 h = 4 weeks 1008 h 6 weeks 1512 h * 9 weeks 2016 h 12 weeks 10. Interpretation of Results 10.1 This practice is intended to simulate the deteriora tion caused by natural weathering. However, the rate of degradation in natural weathering varies from year to year. Laboratory accelerated weathering is more consistent in rate. Therefore, in comparing natural and laboratory weathering one should not attempt to predict the number of hours of laboratory exposure that might equal a year of natural weathering. Even if the details of the natural exposure are fully reported as required by 5.3, any time to time compar ison would apply only to a given year at a particular site. 10.2 It is possible to correlate the deterioration resulting from a period of natural weathering, such as 1 year, to the deterioration resulting from a period of laboratory acceler ated weathering. Spearman rank correlation, which is dis- ' cussed in most basic statistical texts, has proved to be a] useful method for this. A minimum of seven variables must i be ranked by both test methods to obtain statistical validity}, from Spearman rank correlation. Ranking 10 to 15 variables :' by both methods will improve the reliability of such correla-, tions. 10.3 It is frequently not possible to predict how many hours or weeks of accelerated testing will yield the best correlation to some period of outdoor testing. Therefore, laboratory tests should be measured periodically, such as weekly or biweekly, so that the correlation coefficient may be-,' calculated at several points during the accelerated test. 11. Report 11.1 The report shall include the following: 11.1.1 Manufacturer and model of fluorescent UV/ condensation apparatus, II. 1.2 Manufacturer's designation for the fluorescent UV lamp, the wavelength <nm) at which peak emission occurs, and the short wavelength'~at which 1 % of peak emission occurs (for example, FS-40 313/280 nm), 11.1.3 Cycle of UV exposure time and temperature, condensation time and temperature (for example 4 h UV/ 60C, 4 h CON/50C), 11.1.4 Total exposure time, 11.1.5 Special conditions of test, such as rotation of test specimens, and 11.2 A sample report form is shown in Fig. 5. The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any Item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision ofthis standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration af a meeting of the responsible technical committee, which you may attend. If you fee! that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.f Philadelphia, PA 19103. 1092 .i i$ -. i !Miit DUP050298270 be a must, tlidity, iables -rrela- Jiany best Jfore, :h as jy be UV/ uv :urs, sion ure, JV/ test RELATED MATERIAL Any documents included in this section that are marked "proposed" are published for information only. They have received the approval of the sponsoring technical committee for publication as "proposed" but have not been officially accepted by the Society. Comments are solicited and should be addressed to ASTM, 1916 Race St., Philadelphia, Pa. 19103. 1 #t : DUP050298271 List by Subjects 1992 ANNUAL BOOK OF ASTM STANDARDS, VOLUME 06.02 P < --P< { 9 ' , R' < , " PG 9 ' s ; C' G G G ' Since the standards in this book are arranged in alphanumerical sequence, no page numbers are given in this list, j The standards listed in italics are related documents included for information only and do not appear in this volume. For List by Subjects of Volumes 06.01 and 06.03, see pp. xxiv and 1100 A complete Subject Index begins on p. 1133 !!D 3619- 77 (1989) D 603"- 66 (1989) D 602-81(1991)" D 1199-86(1991)" D 604-81(1989) D 605-82(1989) D 867-81(1986)" &D 607 - 82(1987)" D 4288 - 83(1989)" D 476 - 84(1989) D 81-87 D 4462 - 85 (1989) D 79-86 D 210-81a(1991)" D 561 -82(1989) D 769-87(1991)" D 209 - 81 (1989) 962-81 (1986)" 267-82 (1987)" 964-65(1989) 912-81 (1986) 9U'-87 520-84(1989) D 963-81 (1986)" D 261 -75(1987)" D 262-81 (1987)" D 212-87 D 263-75 (1987) D 3021-82 (1987)" D 1649-82 (1987)" D 478-86(1991)" D 211 -67(1989)" D 768-81 (1987)" PIGMENT SPECIFICATIONS Inert or Low Hiding Pigments Aluminum Silicate (Anhydrous) Aluminum Silicate (Hydrous) Barium Sulfate Calcium Carbonate Diatomaceous Silica Magnesium Silicate (Talc) Pumice Wet Ground Mica White Pigments Calcium Borosilicate Titanium Dioxide White Basic Lead Carbonate Zinc Hydroxy Phosphite Zinc Oxide ' Bone Black Carbon Black Iron Oxide, Synthetic Black Lampblack Black Pigments Bronze and Miscellaneous Metallic Pigments Aluminum Powder and Paste Bronze Powder, Gold Copper Powder, Antifouling Cuprous Oxide, Antifouling Mercuric Oxide, Antifouling Zinc Dust Copper Phthalocyanine Blue Iron Blue Ultramarine Blue Blue Pigments Chrome Green Chrome Oxide Green Phthalocyanine Green Green Pigments Yellow, Orange, Brown Pigments Chromate, Strontium Chromate, Zinc Yellow Chrome Yellow and Chrome Orange Iron Oxide, Hidrated Yellow Approved for use by agencies of the Department of Defense and, if indicated on the standard, replaces corresponding Federal or Military document. Consult the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department of Defense. 3095 DU P050298272 D 3722-82 (1991)" D 3724 - 82 (1987)" D 2218-67(1989)" D 85-87(199!)" D 765-87(1991)" D 1648 -86 D 763-81 (1988)" D 3722-82 (1987)" D 3721 -83(1991)" D 475-67(1989) D 83-84(1989) D 656-87 Test Methods for D 305 - 84(1990)" D 480-88 D 718-86(1991)" D 23:50-90 D 715-86(1991)" D 1135-86(1991)" 04487-90 D 126 - 87(1991)" D 185-84(1989)" 0 1208 - 84(1989)" D 283-84(1990)" D 3872-86 (1991)" D 280-81 (1987) D4358 - 84 (1990)" D 717-86(1991)" D 284-88 D 716 - 86(1991)" D3256 - 86 (1993)** D 49-83(1990)" D 970-86(1991)" D 719-86 D 1844-86(1991)" D 1845-86 (1991)" D 2351 -90 D2352- 85 (1990)" D 3720 - 84 D 3926-80 (1991)" D 2742-79 D 2448-85 (1989) D 1301-91 D 1394-76(1991)" D 3280-85 (1990)" D 50-90 D 521-81 D 4450 - 85 (1990)" D 444 - 88 Practice for: D 34-91 Guide for: D4139 -82 (1991)" Test Methodsfor: D 1155-89 D 1214-89 D 1483 - 84(1989)" LIST BY SUBJECTS, VOLUME 06.02 Iron Oxide, Natural Red and Brown Iron Oxide, Synthetic Brown Molybdate Orange Ochre Sienna, Raw and Burnt Silicochromate, Basic Lead Umber, Raw .and Burnt Red Figments Iron Oxides, Natural Red and Brown Iron Oxide, Synthetic Red Para, Pure Red Toner Red Lead Toluidine, Pure Red Toner PIGMENT TEST METHODS Analytical Tests Acetone Extract in Black Pigments, Determination of Aluminum Powders and Pastes, Flaked, Sampling and Testing Aluminum Silicate Pigment, Analysis of Antimony Oxide in White Pigment Separated from Solvent-Reducible Paints, Determination of Barium Sulfate Pigment, Analysis of Blue Pigments, Chemical Analysis of Calcium Borosilicate, Analysis of Chromium, Yellow, Orange, and Green Pigments, Analysis of Coarse Particles in Pigments, Pastes, and Paints Common Properties of Certain Pigments Copper and Dry Cuprous Oxide Pigments, Chemical Analysis of Ferrous Iron in Iron Oxides, Determination of Hygroscopic Moisture (and Other Volatile Matter) in Pigments Lead and Chromium in Air Particulate Filter Samples of Lead Chromate Pigment Dusts Magnesium Silicate Pigment, Analysis of Mercuric Oxide Pigment, Chemical Analysis of Mica Pigment, Evaluating Phthalocyanine Blue and Green Pigments, Chemical Analysis of Red Lead, Chemical Analysis of Red Pigments, Para and Toluidine Silica, Diatomaceous Pigment, Analysis of Silicochromate, Basic Lead, Chemical Analysis of Strontium Chromate Pigment, Chemical Analysis of Sulfide Sulfur in White Pigment Separated from Solvent-Reducible Paints, Determination of Sulfur Dioxide in White Pigment Separated from Solvent-Reducible Paints, Determination of Titanium Dioxide Pigments, Ratio of Anatase to Rutile by X-Ray Diffraction Titanium Dioxide Slurries, Percent Solids in Tribasic Lead Phosphosilicate, Chemical Analysis of (Discontinued I990f) Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of the Pigment White Lead Pigments, Chemical Analysis of White Titanium Pigments, Chemical Analysis of ' White Zinc Pigments, Chemical Analysis of Yellow, Orange, Red, and Brown Pigments, Chemical Analysis of Zinc Dust, Chemical Analysis of Zinc Hydroxy Phosphite, Analysis of Zinc Yellow (Zinc Chromate), Chemical Analysis of White Pigments, Chemical Analysis of Volatile and Nonvolatile Content of Pigments, Determining General Physical Tests Glass Spheres, Routtdness Glass Spheres, Sieve Analysis Oil Absorption of Pigments by Gardner-Coleman Method t Although this standard has been officially withdrawn from Society approval, a brief description is included for information only. 1096 DUP0502 98273 Test Methodsfor: D 281 -84(1989) D 3360 -80 (1989) D 153-84(1989)ei Practice for: D 1366 -86 (1991)41 Test Methodsfor: D 279 - 87 (1991)CI D 3022-84(1989)" D 387 - 86 D 2745-89 D 332 -87 (1991){1 Specificationsfor: D 207-55(1987) D 784-83(1987) D 237-91 D' 360 - 89 Guide for: D4277 -83(1988)1 D 4142-89 D4143-89 D 4368-89 Test Methodsfor: D 1979-91 D 29 - 81 (1987)fl D 365-84(1989)el D 411-83(1987) D 1650-91 D1439-83a (1989)" D 509 - 70(1987) Practicefor: D 2689-88 Test Methods for: D 1926-89 D 2455-89 D 1726-90 D 1847-87 D 1652-90 D 1398-84 D 1615-60(1987) D 2572 - 91 D 2690-89 D 1013-88 D 4613 -86 (1990)" D 1312- 56(1987)" D 4706-87 D 563-88 D 1306-88 D 1396- 73 (1987)" D 3680-89 D 1469 - 73 (1988)" D 1542 - 60(1988)" D 3733 - 78(1984)" D 1397-88 D 465-82(1987 D 1063 - 51(1987) D 1585 - 82 LIST BY SUBJECTS, VOLUME 06.02 Oil Absorption of Pigments by Spatula Rub-Out Particle Size Distribution of Common White Extender Pigments Specific Gravity of Pigments Particle Size Characteristics of Pigments, Reporting Color and Opacity Tests Bleeding of Pigments Color and Strength of Color Pigments by Use of a Miniature Sandmill Color and Strength of Color Pigments with a Mechanical Muller Tinting Strength of White Pigments, Relative, by Reflectance Measurements Tinting Strength of White Pigments, Relative, by Visual Observation RESINS AND POLYMERS Lac, Dry Bleached Orange Shellac and Other Indian Lacs for Electrical Insulation Orange Shellac and Other Lacs Shellac Varnishes General Amino Resins, Testing Epoxy Resins, Testing Latex Vehicles, Testing PolyCVinyl Chloride) Resins, Testing Amino Resins, Free Formaldehyde Content Lac Resins, Sampling and Testing Nitrocellulose Base Solutions, Soluble Shellac for Electrical Insulation, Testing Shellac Varnish, Sampling and Testing Sodium Carboxymethylcellulose Rosin, Sampling and Grading (see Vol 06.03) Alkyd Resins, Testing Resin Chemical Tests Carboxyl Content of Cellulose Carboxylic Acids in Alkyd Resins . ._ Chlorine Content, Hydrolyzable, in Epoxy Resins Chlorine Content, Total, in Epoxy Resins Epoxy. Content of Epoxy Resins Fatty Acids in Alkyds Glycerol, Glycol, and Pentaerythritol in Aikyds Isocyanate Groups in Urethane Materials or Prepolymers Isophthalic Acid in Alkyd and Polyester Resins Nitrogen, Total, in Resins and Plastics pH, Apparent of Water-Insoluble Phenol-Formaldehyde Resins Phenol, Free, in Phenolic Resins Phenolic Resins, Determining Methylol Group Qualitatively in Phthalic Anhydride Content of Alkyd Resins and Resin Solutions Phthalic Anhydride in Alkyds and Esters Containing Other Dibasic Acids (Gravimetric) Poly(Vinyl Butyral), Chemical Analysis of Vinyl Chloride Monomer, Residual Content of Poly(VinyI Chloride) Resins, Compounds,and Copolymers by Solution Injection Technique Rosin Acids Content of Coating Vehicles, Total Rosin in Varnishes, Qualitative Detection Silicon Content of Silicone Polymers and Silicone-Modified Alkyds by Atomic Absorption Unsaponifiable Matter in Alkyds, Vinyl Chloride Acid Number ofRosin (see Vol 06.03) Ash in Rosin (see Vol 06.03) Fatly Acids in Tall Oil Rosin (see Vol 06.03) 1097 ` S'. DUP050298274 LIST BY SUBJECTS, VOLUME 06.02 Test Methods for: D 1064 - 58(1981) D 464-91 D1065 -82 Iron in Rosin (see Vol 06.03) Saponification Number ofRosin (see Vol 06.03) Unsaponifiabie Matter in Rosin (see Vol 06.03) ology of 1695-77 Test Methods for: D 2090 - 88 D 1544-80 (19S9)1 Color Tests Clarity and Cleanness of Paint and Ink Liquids Color of Transparent Liquids (Gardner Color Scale) iethodsi 3536 - 76, 3593 -- Resin Physical Tests Test Methodsfor: D 5097 - 90 D 4758 - 87 D 1259 - 85 (1990)tl D 4613 - 86 D4640-86(1990)ei D 4639-86(1990)*1 D 2998 - 89 D 2456 - 91 D 3432 - 89 D 4827 - 88 D4747 - 87 ' D 3008 - 90 28-67 (1982)*' D 889 - 58(1987) Filter-Retained Solids Content of Polymer Latexes Nonvolatile Content of Latexes / ticesfor: >3750 - 7% Nonvolatile Content of Resin Solutions pH, Apparent, of Water-Insoluble Phenol-Formaldehyde Resins Phenol-Formaldehyde Resins, Determining Stroke Cure Time of Thermosetting >2857-8 >4001-8 Phenolic Resins Volatile Content Polyhydric Alcohols in Alkyd Resins, Determination of Polyhydric Alcohols in Alkyd Resins, Identification of : cificationj) Toluene Diisocyanates, Unreacted, in Thermosetting LIrethane Prepolymers and Coating Solutions UsinJ io o -I Gas-Liquid Chromatography ,, _ .. Unreacted Monomer Content of Latexes Using Capillary Column Gas Chromatography Unreacted Monomer Content of Latexes Using Gas-Liquid Chromatography Resin Acids in Rosin by Gas Chromatography (see Vol 06.03) 133-fi 11-;8' Softening Point by Ring- and Ball-Apparatus (see Vol 06.03) Method Volatile Oil in Rosin (see Vol 06.03) 70 -*f Practice for: D4209-82 (1991)el Test Methodsfor: D'3132 - 84 (1990)EI D 1198-88 D 269 - 52 (1987)ej Volatile and Nonvolatile Content of Cellulosics, Emulsions, Resin Solutions, Shellac, and Varnishes Solubility and Miscibility Tests Solubility Range of Resins and Polymers Solvent Tolerance of Amine Resins ,, Toluene-Insoluble Solid Mailer in Rosin (Chiefly Sand, Chips, Dirt, and Bark) (see Vol 06.03) Definitions dices fof. <5166-1 300 -| 20hi 180 -| 200 ,, , 'I yimtions.i IE 12-1- Definitions of Terms Relating to: D 804 - 79(1987) Test Methodsfor: Naval Stores and Related Products (see Vol 06.03) CELLULOSE AND CELLULOSE DERIVATIVES Ucticefor, |' 386 ' D 1794 -89 D 3516 -89 D 1926 -89 D 817 -91 D 871 -91 D 1716 - 62(1987) D 301 -89 D 2641 -89 D 1915 - 63 (1989)l D 3971 -89 D 4794 -88 D 914 -72(1989)*1 D 2364 -89 D 2363 - 79 (1989)el D 1795 -90 D 4085 -81 (1987) D 3876 - 79 (1989)*' D 1347 -72 (1989)ei D 1348 -89 D 4795--88 D 1787 -89 D 2438 -89 D 1439 - 83a (1989)* D 1696 -90 D 2929 -89 D 1343 -91 Alcohol-Benzene Soluble Matter in Cellulose (Intent to Withdraw) Ashing Cellulose Carboxyl Content of Cellulose Cellutose Acetate Propionate and'Cellulose Acetate Butyrate, Testing Cellulose Acetate, Testing ------ - Cellulose Chain Length Uniformity by Fractional Precipitation of Cellulose Nitrate Cellulose Nitrate, Soluble Chlorine in Cellulose Chromatographic Analysis of Chemically Refined Cellulose Dichloromethane-Soluble Matter it) Cellulose Ethoxyl Substitution in Cellulose Ether Products by Gas Chromatography, Determination of Ethylcellulose ...... , Hydroxyethylcellulose Hydroxypropyl Methylcellulose Intrinsic Viscosity of Cellulose Metals in Cellulose by Atomic Absorption Spectrophotometry Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography Methylcellulose Moisture in Cellulose Nitrogen Content of Soluble Nitrocellulose--Alternative Method Pentosans in Cellulose Silica in Cellulose Sodium Carboxymethylcellulose Solubility of Cellulose in Sodium Hydroxide Sulfur Content of Celiulosic Materials by X-ray Fluorescence Viscosity of Cellulose Derivatives by Ball-Drop Method F i 1098 DUP050298275 LIST BY SUBJECTS, VOLUME 06.02 Terminology of: D 1695 - 77 (1989)< Cellulose and Cellulose Derivatives POLYMERS ,Test Methods for: D 3536 - 76 (]988)<LI D 3593 -- 80 (1-986f! .Molecular Wdight Averages'and Molecular Weight Distribution bp Liquid Exclusion Chromatography (Gel Permeation Chromatography--GPC) (see Vol 08.03) Molecular, Weight Averages and Molecular Weight Distribution of Certain Polymers by Liquid Size- Exclusion Chromatography (Gel Permeation Chromatography--GPC) Using Universal Calibration (see Vol 08.03) Practices for: D 3750 - 79(1985) D 2857 - 87 D 4001 - 81 (I986)t! Number-Average Molecular Weight of Polymers by Membrane Osmometry, Determination -of (see Vol 08,03). ... . . Viscosity ofPolymers, Dilute Solution'(see Vol 08.02) Weight-Average Molecular Weight ofPolymers by Light Scattering, Determination of(see Vol 08.03) GENERAL STANpARDS Specificationsfor: E 100 - 81(1986} E 1-90 E 133-86 E 11-87 ASTM Hydrometers (see Vol 14.03) ' ASTM Thermometers (see Vol 14.03) .* Distillation Equipment (see Vol 14.02) Wire-Cloth Sieves for Testing Purposes (see Vols 04.01, 04.02, 04:06, 05.05, and 14.02) Test Methods for: E 70-90 pH ofAqueous Solutions with the Glass Electrode (see Vol 15.05) Practices for: D 5166-91 E 300 - 86 E 20-85 E 180-90 E 200 - 86 Gelled Vehicle Samples, Laboratory Preparation Using a Microwave Oven Industrial Chemicals, Sampling (see Vol 06 03) Particle-Size Distribution of Particulate Substances of Subsieve Sizes, [Analysis by Microscopical Methods for (see Vol 14.02) , Precision ofASTM Methodsfor Analysis and Testing ofIndustrial Chemicals', Developing (see Vol 15(05) Standard Solutionsfor Chemical Analysis, Preparation, Standardization, and Storage of(see Vol 15.05) Definitions of Terms Relating to: :" E 12-70(1986) Density and Specific Gravity of Solids, Liquids, and Gases (see Vols 04.02 and 15,05) METRIC PRACTICE Practice for: E 380-91 Use of the International System of Units '(SI) (the Modernized Metric System) (Excerpts) (see Related Material section) 1099 DUP050298276 List by Subjects . 1992 ANNUAL BOOK OF ASTM STANDARDS, VOLUME 06.03 P < --F O< G " A( < " , N G S' , SG ' n t s , M< ( ' G G ' ; A!"9 #< ( H$"%&( %' &'s Since the standards in this book are arranged in alphanumerical sequence, no page numbers are given in this list. The standards listed in italics are related documents included for information only and do not appear in this volume. For List by Subjects of Volumes 06.01 and 06.02, see pp. xxiv and 1095 A complete Subject Index begins on p. 1133 Specifications for: D 1539 60(1988) D 961 86 D 960 79(1988) D 1841 63(1988)*' D 1842 63(1988) D 1843 63 (1988)t D 1538 60(1988)*' D 260 86(1990) D 234- 82 (1991)eI D 601- 87 (1991)*' D1392- 87 D 1537 - 60(1988)*' D 124- 88 D 1462- 87 D3169- 89 D 1984- 69(1988) D 12- 88 Test Methods for: D 1950 -86 D 1980-87(1991) D 1951 t 86 01952 - 86 D 2090 - 88 D 1967-86 D 1981 -86(1990) D 1544-80 (1989)*' . D 1358 -86 D 1983-90 D 3457-87 (1991)*' D 2800 - 87 D3725-78(1988)*' D 93 - 90 D 3278 - 89 0 1966 - 69(1991)*' D 1954 - 86 D 1955 -85 (1989)*' D 1957-86 D 2245-90 D 1959-85 (1989)*' D 1541 -86 FATTY OILS AND ACIDS, DRYING AND NONDRYING Castor Acids, Dehydrated Castor Oil, Dehydrated Castor Oil, Raw Coconut Fatty Acids, Distilled Com Fatty Acids, Distilled Cottonseed Fatty Acids, Fractionated and Distilled Linseed Fatty Adds, Distilled Linseed Oil, Boiled Linseed Oil, Raw Oiticica Oil (Permanently Liquid) Safflower Oil Soybean Fatty Acids, Distilled Soybean Oil, Degummed Soybean Oil, Refined Sunflower Oil Tall Oil Fatty Acids Tung Oil, Raw Acetone Tolerance of Heat-Bodied Drying Oils Acid Value of Fatty Acids Ash in Drying Oils and Fatty Acids Break in Drying Oils, Quantitative Determination of Clarity and Cleanness of Paint and Ink Liquids Color After Heating of Drying Oils (Heat Bleach), Measuring Color After Heating of Fatty Acids, Measuring Color of Transparent Liquids (Gardner Color Scale) Diene Value, Spectrophotometric, of Dehydrated Castor Oil and Its Derivatives Fatty Acid Composition by Gas-Liquid Chromatography of Methyl Esters Fatty Acid Composition by Gas-Liquid Chromatography, Preparation of Methyl Esters from Fatty Acids for Determination of Fatty Acid Composition by Gas-Liquid Chromatography, Preparation of Methyl Esters from Oils for Determination of Fish Oil in Drying Oils and Drying Oil Fatty Acids by Gas-Liquid Chromatography, Semiquantitative Determination of Flash Point by Pensky-Martens Closed Tester Flash Point of Liquids by Setaflash Closed-Cup Apparatus Foots in Raw Linseed Oil (Gravimetric Method) Foots in Raw Linseed Oil (Volumetric Method) Gel Time of Drying Oils Hydroxyl Value of Fatty Oils and Acids Identification of Oils and Oil Acids in Solvent-Reducible Paints Iodine Value of Drying Oils and Fatty Acids Iodine Value, Total, of Drying Oils and Their Derivatives Approved for use by agencies of the Department of Defense, and if indicated on the standard, replaces corresponding Federal or Military document. Consult the DoD Index of Specifications and Standards for the specific year of issue which has been adopted by the Department of Defense. 1100 DUP050298277 W Methodsfor: DI960 - 86 (1990) ,'D 1958 86 (1990) D 2575 70(1987) |D 1240- 82 D1466 - 86 > 1962- 85 (1989)*1 D1963 - 85 (1989)ei I" 803- 82(1987) I" 1585- 82 D 1982- 85 (1989)1 ~D 1964- 85 (1989)f 1 "D 1965 - 87 (199l)l D 1545 - 89 ruidesfor: |" 555 - 84 (1988)61 D 1467 - 89 D4140- 82 (1991)l est Methodsfor: D 2076 - 64 (1987)ei D2074-66(1987)CI D2073-66(1987)e> D 2077-64 (1987) D 2071 -87(1991) D 2075 - 89 D 2078-86 (1990) D 2080-64 (1987) D 2082 -82 (1987) 02079-82(1987) D208I -64(1987) D 2083-66 (1987) D2072-66(1987)fI D 235 - 871 D 3735 - 87 D 13-82 (1987) D- 836 - 84 D 835-85 D 2359-85a D 3055-86 D 3734-91 D4077-81 (1986)` D2827 - 88el D 362-84 D 841-85 D 4076 - 86 D 843 - 80 (1985)1 D 846 - 84 D 319-90 D 330-89 D 304-90 D 1007 - 85 D 2694-87 D 2696-87 D 4836-90 D 331-90 LIST BY SUBJECTS, VOLUME 06.03 Loss on Heating of Drying Oils Oiticica Oil, Chloroform Insoluble Matter in Polymerized Fatty Acids Rosin Acids in Fatty Acids Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Related Materials Saponification Value of Drying Oils and Fatty Adds Specific Gravity of Drying Oils, Varnishes, Resins, and Related Materials Tall Oil Tall Oil Rosin, Fatty Acids Content of Titer of Fatty Acids Tung Oil Quality Unsaponifiable Matter in Drying Oils and Fatty Acids Viscosity of Transparent Liquids by Bubble Time Method Drying Oils, Testing Fatty Adds Used in Protective Coatings, Testing, Volatile and Nonvolatile Content of Driers, Drying Oils, Naval Stores, and Solvents, Determining FATTY NITROGEN PRODUCTS Acid Value and Amine Value of Fatty Quaternary Ammonium Chlorides Amine Values, Total, Primary, Secondary, and Tertiary, of Fatty Amines by Alternative Indicator Method Amine Values, Total, Primary, Secondary, and Tertiary, of Fatty Amines, Amidoamines, and Diamines by Referee Potentiometric Method Ash in Fatty Quaternary Ammonium Chlorides Fatty Nitrogen Products Iodine Value of Fatty Amines, Amidoamines, and Diamines Iodine Value of Fatty Quaternary Ammonium Chlorides Molecular Weight, Average, of Fatty Quaternary Ammonium Chlorides Non-amines, Percent in Fatty Nitrogen Compounds Nonvolatile Matter (Solids) in Fatty Quaternary Ammonium Chlorides pH of Fatty Quaternary Ammonium Chlorides Primary, Secondary, and Tertiary Amines, Percent in Fatty Amines Water in Fatty Nitrogen Compounds SOLVENT SPECIFICATIONS Petroleum Spirits Petroleum Spirits (Mineral Spirits) VM&P Naphthas Turpentine, Spirits of Terpene Solvents ' '' Aromatic Hydrocarbons and Related Materials Benzene! Industrial Grade (Discontinued 1991) Benzene-485, Refined (Nitration Grade) Benzene-535, Refined Cyclohexane 995 High-Flash Aromatic Naphthas Isopropylbenzene (Cumene) Styrene Monomer 996 Toluene, Industrial Grade (Discontinued 1991) Toluene, Nitration Grade c-Xylene 950 Xylene, Nitration Grade Xylene, Ten-Degree (Discontinued 1991) Alcohols and Ether Alcohols Amyl Alcohol (Synthetic) 2-Butoxyethanol n-Butyl Alcohol (1-Butanol) sec-Butyl Alcohol (2-Butanol) Diethylene Glycol Dipropylene Glycol (Discontinued 19921--Replaced by Specification D 5164) Dipropylene Glycol Monomethyl Ether 2-Ethoxyethanol 1101 DU P05 02 982 78 D 2693 - 87 D 2636 -91 D 1719-90 D 770-90 D 3160 - 91 D 3128-89 D 1152-89 D2635-9I D 3622 - 90 D2695-87 D 4837-89 D 329 - 90 P 2627 -91 D 2916 - 88 D 4360 - 90 D 740 - 89 D 3729 - 84 D 2917-91 D 1153 - 90 D 3540-86 D4615 -86" D 3728-88 D 4614 - 86 D 5137-90 D 1718-86 D3131 -88 D 2634-86 D 3130 - 86 D 4835-89 Test Methods for D 801 -57(1987) D 233 -65 (1981)" D 268-90 Test Methodsfor D 1612-90 D 1613-91 D 847-87 D 1614-91 D 1492 - 87 D 2324-81 (I989)ei D 848-81 (1989)61 D 849-88 D 130-88 D 1617-90 D 853-82(1987)" D 1363 -88 D 3961 -89 D 1685-86 D 890-58(1987) D 1364-90 E 203 - 75 (1986)fI Test Methodsfor: D 3545 - 90 LIST BY SUBJECTS, VOLUME 06.03 Ethylene Glycol Hexylene Glycol Isobutyl Alcohol (Isobutanol) Isopropyl Alcohol (Isopropanot) Isopropylbenzene (Cumene), Phenol Content 2-Methoxyethanol Methanol (Methyl Alcohol) Methyl Isobutyl Carbinol ri-Propyl Alcohol (I-Propanol) Propylene Glycol (Discontinued 1992)--Replaced by Specification D 5164) Propylene Glycol Monomethyl Ether Ketones Acetone Diacetone Alcohol ' ' Isophorone Methyl -Amyl Ketone Methyl Ethyl Ketone Methyl Ethyl Ketone (99.5 % Grade) (Discontinued 1989f--Replaced by Specification D 740) Methyl Isoamyl Ketone Methyl Isobutyl Ketone Esters Amyl Acetate, Primary, Synthetic (98 % Grade) n-Butyl Acetate (All Grades) 2-Ethoxyethyl Acetate (99 % Grade) Ethyl Acetate (All Grades) Hexyl Acetate Isobutyl Acetate (95 % Grade) Isopropyl Acetate (98 % Grade) Methyl Amyl Acetate n-Propyl Acetate (96 % Grade) Propylene Glycol Monomethyl Ether Acetate SOLVENT TEST METHODS General Methods Dipentene, Sampling and Testing Turpentine, Sampling and Testing Volatile Solvents for Use in Paint and Related Coatings and Materials, Sampling and Testing Chemical Tests Acetone in Methanol (Methyl Alcohol) Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related Products Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aromatic Hydrocarbons Alkalinity in Acetone Bromine Index of Aromatic Hydrocarbons by Coulometric Titration Carbon Disulfide in Benzene Color, Acid Wash, of Industrial Aromatic Hydrocarbons Copper Corrosion by Industrial Aromatic Hydrocarbons Copper Corrosion from Petroleum Products Ester Value of Lacquer Solvents and Thinners Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons Permanganate Time of Acetone and Methanol Sulfur, Trace Quantities in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry Thiophene in Benzene, Traces of. Using Isatin and Spectrophotometry Water in Liquid Naval Stores Water in Volatile Solvents (Fischer Reagent Titration Method) Water Using Karl Fischer Reagent (see Vo! ]5.05) Physical Tests Acetate Esters, Alcohol Content and Purity by Gas Chromatography DeftnitiJp D 80s; t Although this standard has been officially withdrawn from Society approval, a brief description! is included for information only. 1102 DUP050298279 LIST BY SUBJECTS, VOLUME 06.03 lated ns s-i; Test Methodsfor: 5 D 3257 --88 ; D 2935 -81 (1985) D 4367 --89 D 1209--84(1988)" ; D 3054 --81(1985) | D 850 -86 D 86--90 D 1078--86 D 5008 -89 SD3539--87 D 3934 --90 D 1310-- 86 (1990)" D 93--90 D 56--87 D3941 --90 D 3278 -82" D 3893 -90 D 2804 --88 D 3329 -- 89 D 2360 - 82(1987)" D4353 - 90 D 1296 -84(1988)" D4773-:89 D 852-87 D 1493 - 84(1988) D 4206 - 89 D 4207 - 91 D 3962 - 80(1989)" I D 3009 - 72(1981)" D 1555- 83 D 95- 83(1990) D2306- 81(1985) D 3797 - 88 D 3798 - 89 D 1217- 86 D1015 - 84 D1016 - 84 D1218 - 87 Aromatics in Mineral Spirits by Gas Chromatography Apparent Density of Industrial Aromatic Hydrocarbons Benzene in Hydrocarbon Solvents by Gas Chromatography Color of Clear Liquids (Platinum-Cobalt Scale) Cyclohexane, Purity and Benzene Content by Gas Chromatography Distillation of Aromatic Hydrocarbons Distillation of Petroleum Products Distillation Range of Volatile Organic Liquids 2-Ethylhexonal, Ethyl Methyl Pentanol Content and Purity Value by Gas Chromatography Evaporation Rates of Volatile Liquids (see Vol 06.01) Flash/No-Flash--Equilibrium Method by a Closed-Cup Apparatus Flash Point and Fire Points of Liquids by Tag Open-Cup Apparatus ' Bash Point by Pensky-Martens Closed Tester Bash Point by Tag Closed Tester Bash Point of Liquids by Equilibrium Method With Closed-Cup Apparatus Flash Point of Liquids by Setaflash Closed-Cup Apparatus Methyl Amyl Ketone and Methyl Isoamy] Ketone Purity by Gas Chromatography Methyl Ethyl Ketone Purity Using Gas Chromatography Methyl Isobutyl Ketone Purity by Gas Chromatography Monocyclic Aromatic Hydrocarbons, Trace Impurities in, by Gas Chromatography Nonvolatile Matter in Volatile Solvents for Use in Paint,^Varnish, Lacquer, and Related Products Odor, Residual, of Volatile Solvents and Diluents Purity of Propylene Glycol Monomethyl Ether, Dipropylene Glycol Monomethyi Ether, and Propylene Glycol Monomethyl Ether Acetate Solidification Point of Benzene Solidification Point of Industrial Organic Chemicals Sustained Burning of Liquid Mixtures by Setaflash Apparatus (Open Cup) Sustained Burning of Low-Viscosity Liquid Mixtures by Wick Test Styrene Analysis by Gas Chromatography Turpentine Composition by Gas Chromatography Volume and Weight of Industrial Aromatic Hydrocarbons, Calculation of Water in Petroleum Products and Bituminous Materials by Distillation Xylene Isomer Analysis by Gas Chromatography oXylene Analysis by Gas Chromatography p-Xylene Analysis by Gas Chromatography Density and Relative Density (Specific Gravity) ofLiquids by Bingham Pycnometer (see Vol 05.01) Freezing Points of High-Purity Hydrocarbons Purity of Hydrocarbons from Freezing Points Refractive Index and Refractive Dispersion ofHydrocarbon Liquids (see Vol 05.01) Solubility and Miscibility Tests Test Methods for: D 611-82(1987)" D 1720 - 88 D 1476 - 88 D 1133-90 D 1722 - 90 Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents Dilution Ratio of Active Solvents in Cellulose Nitrate Solutions Heptane Miscibility of Lacquer Solvents Kauri-Butanol Value of Hydrocarbon Solvents Water Miscibility of Water-Soluble Solvents ___ Liquid Naval Stores Test Methodsfor: D 801 -57 (1987) D 86 - 82 D 56-87 D 802-82(1987) D 856-49(1987) D 1131 - 53(1981)" D 803-82(1987) D 233-65 (1981)" D3009 -72 (1981)" D 890-58(1987) Dipentene, Sampling and Testing Distillation of Petroleum Products Bash Point by Tag Closed Tester Pine Oil, Sampling and Testing Pine Tars and Pine-Tar Oils Rosin Oils Tali Oil Turpentine, Sampling and Testing Turpentine Composition by Gas Chromatography Water in Liquid Naval Stores General Definitions of Terms Relating to: D 804 - 79 (1987) Naval Stores and Related Products 1103 ..... DUP050298280 LIST BY SUBJECTS, VOLUME 00.03 Specificationsfor D 4710-87 D 3620-90 D4416-89 D 3547 - 91 D 608-90 D 3548 - 86 D 3193 - 91 D 3541 -91 D 1969 - 91 D2378 - 84 (1987) D 1257-90 D 3504-91 D 3845-89 D 4709-87 D 600-90 D2403-68(1982) D 363-90 D 2190 -89 Test Methods for: D 3362-84 (1987) D4415-91 D 2192-89 D 2119 - 87 D2613-85 (1990) D 3970-80 (1990) D2373 - 85 (1990) D 2379-84 (1987) D2194-89 D 2087 - 89 D 2380-84 (1987) D 3546 -90 D 1258 - 90 D 1728-83 D 3804 - 86 (1991)el D 2374-85 (1990) D 2375 -85 (1990)el D 3125-83 (1987) - D 2999-85 D 564-87 (1991) D 2195 -84 D 3989- 81a (1990)" D 3962 - 80 (1984)e 1 D 2119-87 D 2120-87 D 2340- 82 (1987) D 2121-84 D 1721 -84(1988) D 1399-90 D 1468 - 84(1988) D 1638 - 74 D 3988 - 85 (1990) D2191 -84 D 2086-84 D2193-84 D 1631-85 D 3969-85(1990) Terminology Relating to: D 16-91 Test Methods for: D 465-82(1987) MISCELLANEOUS RAW MATERIALS Acetaldehyde Acetic Acid, Glacial Acrylic Acid n-Butyl Acrylate Dibutyl Phthalate Ethyl Acrylate Ethylbenzene 2-Ethylhexyl Acrylate 2-Ethylhexyl (Synthetic) Formaldehyde Glycerin, High-Gravity Maleic Anhydride Methacrylic Acid, Glacial Methyl Acrylate Paint Driers, Liquid Phthalic Anhydride-1308, Refined Tricresyl Phosphate Vinyl Acetate Acrylate Esters, Purity by Gas Chromatography Acrylic Acid, Determination of Dimer in Aldehydes and Ketones, Purity of Aldehydes in Styrene Monomer ! Calcium and Zinc in Paint Driers,by EDTA Method ' Cerium in Paint Driers by Oxidimetric Determination Cobalt in Paint Driers by EDTA Method Formaldehyde Solutions, Acidity of Formaldehyde Solutions, Concentration of . Formaldehyde Solutions; Iron iri; x Formaldehyde Solutions, Methanol Content of Formic Acid'in Glacial Acetic Acid.. ' Glycerin, High-Gravity, Testing Glycerin, Phthalate Ester Color of High Gravity (Discontinued 199 It) ' Iron in Paint Driers by EDTA Method `, Lead in Paint Driers by EDTA Method ' Manganese in Paint Driers by EDTA Method ' '' Monomethyl Ether of Hydroquinone in Colorless Monomeric Acrylate Esters and Acrylic Acid Monopentaerythritol in Commercial Pentaerythritol by Gas Chromatography (Discontinued Replaced by Test Method D 2195) Paint Driers, Liquid Pentaerythritol Rare Earth Metals, Total, in Paint Driers by EDTA Method; ' ; Styrene Analysis by Gas Chromatography . Styrene Monomer, Aldehydes in _ Styrene Monomer, /Hert-Butylcatechol Inhibitor in Styrene Monomer, Peroxides in Styrene Monomer, Polymer Content of Tricresyl Phosphate, Permanganate Time of Tricresyl Phosphate, Unsaponifiable Content of Tricresyl Phosphate, Volatile Matter in Urethane Foam Isocyanate Raw Materials (Discontinued 1991 f) Vanadium in Paint Driers by EDTA Method Vinyl Acetate, Acetaldehyde Content of Vinyl Acetate and Acetaldehyde, Acidity in Vinyl Acetate, Hydroquinone in Water in Phenol and Related Materials by the Iodine Reagent Method Zirconium in Paint Driers by EDTA Method Paint, Varnish, Lacquer, and Related Products NAVAL STORES Rosin Acid Number of Rosin 1104 DUPO 502 98281 rest Methodsfor: D 1063-51(1987) ,D 1585-82 D 1064-58(1981) D 3008 -90 D 1240-82 ID 509-70(1987) ^ D 464-91 E 28 -- 67 (1982)el D 269 - 52 (1987)ei D 1065-82 D 889-58(1987) j Specifications for: D 3264 - 86 D 836-84 ' D 835-90 \ \ D 2359-90 : D 4734 90 I D 3055-90 ! D 4077-91 D 3504-87 D2439-91 D 2403-91 D 2323-84 (1989)" D 2827-88" :D 362-84 D 841-90 D 5211 -91 D 843-90 D 846-84 D 4076-86 (1990) D 5136-90 jTest Methods for: D 847- 91 D 848- 81(1989)" D2I19- 87 D 2935 - 91 D4492- 85(1989)" D 4534 - 89 D 1492- 91 D 2324 - 81(1989)" D 5194 - 91 D 3627 - 82(1987)" D4789"- 88 D 3366 - 90 D 1686- 81 (1990) D 4590 - 86 D 849- 88 D 3439 - 89 D3505 - 84" D 850- 91 D 2232 - 81 (1986)" D1015 - 89 D 2870 - 86 D 853 - 91 D 5060 - 90 D 4961 - 89 D2120- 87 D 3760 - 79(1984) D 2930 - 80(1989)" D 2360- 82 (1987)" D4589- 91 D 2340 - 82(1987)" D 2121 - 90 LIST BY SUBJECTS, VOLUME 06.03 Ash in Rosin Fatty Acids Content of Tall Oil Rosin Iron in Rosin Resin Acids in Rosin by Gas Chromatography Rosin Acids in Fatty Acids Sampling and Grading Rosin Saponification Number of Rosin Softening Point by Ring-and-Ball Apparatus Toluene-Insoluble Solid Matter in Rosin (Chiefly Sand, Chips, Dirt, and Bark) Unsaponifiable Mattel in Rosin Volatile Oil in Rosin AROMATIC HYDROCARBONS AND RELATED MATERIALS (see gray-edge pages 523 to 797 of Volume 06.03) Aniline, Industrial Grade Benzene, Industrial Grade (Discontinued I991f) Benzene-485, Refined (Nitration Grade) Benzene-535, Refined Benzene-545, Refined Cyclohexane 995 Isopropylbenzene (Cumene) Maleic Anhydride Phenol, Refined Phthalic Anhydride-1308, Refined Pyridine, Refined Styrene Monomer 996 Toluene, Industrial Grade (Discontinued 199If) Toluene, Nitration Grade Xylene, Feedstock for p-Xylene Xylene, Nitration Grade Xylene, Ten-Degree (Discontinued 199If) oXylene 950 p-Xylene, High Purity Acidity of Benzene, Toluene, Xylenes, Solvent Naphthas, and Similar Industrial Aromatic Hydrocarbons Acid Wash Color of Industrial Aromatic Hydrocarbons Aldehydes in Styrene Monomer Apparent Density of Industrial Aromatic Hydrocarbons Benzene Analysis by Gas Chromatography Benzene Content of Cyclic Products by Gas Chromatography Bromine Index of Aromatic Hydrocarbons by Coulometric Titration Carbon Disulfide in Benzene Chloride, Trace, in Liquid Aromatic Hydrocarbons Color of Cresylic Acids ("C" Series Standards) Color of 4,4'-Isopropylidenediphenol (Bisphenol A) in Solution -- Color of Maleic Anhydride and Phthalic Anhydride in the Molten State and After Heating Color of Solid Aromatic Hydrocarbons and Related Materials in the Molten State (Platinum-Cobalt Scale) Colorimetric Determination ofp-terh-Butylcatecbol in Styrene Monomer by Addition of Alcoholic NaOH Copper Corrosion of Industrial Aromatic Hydrocarbons Cresylate Solutions, Alkaline, from Petroleum Sources Density or Relative Density of Pure Liquid Chemicals Distillation of Industrial Aromatic Hydrocarbons and Related Materials Evaporating Residue of Naphthalene Freezing Points of High-Purity Hydrocarbons Gel Time of Tar Acids Hydrogen Sulfide and Sulfur Dioxide Content (Qualitative) of Industrial Aromatic Hydrocarbons Impurities in High-Purity Ethylbenzene by Gas Chromatography, Determing Impurities, Major Organic, in Phenol Produced by the Cumene Process by Gas Chromatographic Analysis Inhibitor, p-tert-Butylcatechol, in Styrene Monomer Isopropylbenzene (Cumene) by Gas Chromatography Maileic Acid in Maleic Anhydride by Potentiometric Titration Monocyclic Aromatic Hydrocarbons, Trace Impurities in, by Gas Chromatography Nitrobenzene in Aniline Peroxides in Styrene Monomer Polymer Content of Styrene Monomer MMIII--i 1105 DUP050298282 LIST BY SUBJECTS, VOLUME 0B.03 Test Methodsfor: D3054-81 (1985) D 1016-89 D447I -85 (1989)fI D 2031 -84(1989)ei D 852-87(1991) D 1493-90 D 4493 - 89 D 5135 - 90 D 3962 - 80 (1989)el D 3799-89 D 3961 -89 D 3626-85 (1990f' 01685-86(1990) D 4735-87(1991 )ei D 1555 - 91 D 1631 -85 (1989)C1 D 2030-84 (1989)l D2306-81 (1985) D 3797 - 88 D 3798-89 D 1217-86 D 1218-87 Purity and Benzene Content of Cyclohexane by Gas Chromatography Purity of Hydrocarbons from Freezing Points Pyridine Bases in Cresylic Acid by Direct Titratimj- Reducing Substances in Refined Pyridine Solidification Point of Benzene; t ; . Solidification Point of Industrial Organic Chemicals. . - ,, Solidification Point of 4,4'-Isopropylidenediphenol (Bisphenol A) ,.i' Styrene, Analysis of, by Capillary Gas Chromatography Styrene, Analysis of, by Gas Chromatography ;(<. .n Styrene Purity by Freezing Point Method Sulfur, Trace Quantities, in Liquid Aromatic Hydrocarbons by Oxidative Microcoulometry Tar Acid Composition by Gas Liquid Chromatography ? Thiophene in Benzene, Traces of, Usingisatin and Spectrophotometry Thiophene in .Refined Benzene, Trace, by Gas Chromatograph ' Volume and Weight of Industrial Aromatic Hydrocarbons,'Calculation of Water in Phenol and Related Materials by the Iodine Reagent Method Water Solubility of Refined Pyridine Xylene Isomer Analysis by Gas Chromatography -Xylene by Gas Chromatography 11 p-Xylene by Gas Chromatography ' ' ` , '> * , Density and Relative Density (Specific Gravity) ofLiquids'byBingham Pycnometer (see Vo! 05.01) Refractive Index and Refractive Dispersion of Hydrocarbon Liquids (sie Vbl 05.01) Practices for: D 3436 -91 D 4297-89 D 3437 -89 D 3438-89 D 3852-90 , !'' .'ll- / Aniline, Sampling and Handling ' 4,4'-Isopropy!idenediphenol (Bisphenol A), Sampling and Handling Liquid Cyclic Products, Sampling and Handling' ' ( ir Naphthalene, Maleic Anhydride, and Phthalic Anhydride, Sampling and Handling Phenol and Cresylic Acid, Sampling and Handling ' r; Guidefor: D 4588-87 p-Xylene, Analysis of (Discontinued 1992+--Replaced by Specification D 5136) Terminology of: D 4790 - 89a Aromatic Hydrocarbons and Related Chemicals GENERAL STANDARDS Specifications for: D1193 - 91 E 100-81(1986) E 1-90 E 133-86 Reagent Water ' ** ASTM Hydrometers (see Vol 14.03) ASTM Thermometers (See Vol 14!03f Distillation Equipment (see Vol 14.02) ' i' ' 'll U .<-nt ' "J* ; ' Test Methods for: E 299-90 E 70-90 E 200 - 86 Peroxides in Organic Solvents, Trace Amounts - ' pH ofAqueous Solutions with the Glass Electrode (See Vol 15.05) --- Standard Solutionsfor Chemical Analysis, Preparation, Standardization, And Storage of(see Vol 15.05) Practices for: E 300 - 86 E 691 - 87 Industrial Chemicals, Sampling ; Interiabo'ratory Study to Determine the Precision of a Test Method, Conducting Definitions of Terms Relating to: ;; .,.u E 12-70 (1986) Density and Specific Gravity ofSolids, Liquids, and Gases (see Vols 04:02 and 15.05) METRIC PRACTICE . Practice for: E 380-91 '" Use of the International*System,.of Units (SI) (the Modernized Metric System) (Excerpts) (see Related Material section) .-i r 106 m .--aiwwj DUP050298283 Excerpts from Standard Practice for Use of the International System of Units (SI) (the Modernized Metric System)1 Following are excerptsfrom Standard Practice for Use ofthe International System of Units (SI) the Modernized Metric System E 380, which is available as a separate publication and which appears in its entirely in Volume 14.02. Deleted are Appendixes X1. X2. X3. and X4. Added is a table ofselected conversion factorsfrom Appendix X3. CONTENTS Section cope........................................... .......................... ................................................................................................................ I Units and Symbols............................................... .............................................................................................................. Classes of Units..................... ........................................................................................................................... .............. Base Units........... ................................................................................................................................................................ Supplementary Units ............................................................ Derived Units .. ..................... .............................................................................................................. ' ......................... SI Prefixes..........................................................................................................................'.................................... ............. Application of the Metric System.................................... ........................................................................................ ........... General ....................................................................... ........................................................................................................ Application of SI Prefixes............................................................................................. ........................................................ Other Units................................................................ ........................... .................. ,........................ ................................. Other. Recommendations Concerning Units.................................................... Style and Usage..................................................................................................................................................................... Rules for Conversion and Rounding ............................... ....................................... ............................................................. General ............................................................................................................... ........................................................... Accuracy and Rounding.................................................................................................... . ..........................................' . . Significant Digits............. ................................... .............................................. :................................................................. Rounding Values............................................ ....................................................................................... ,............................ Conversion of Linear Dimensions of Interchangeable Parts..................................................................... ........... ............... Other Units ;................................. '..................... ............................................ :.................. ................................................ Terminology ......................................'.......................................................................................................'........................... Appendixes Development of the International System of Units................................................................................................................ Organs of the Metre Convention: BIPM, CIPM, CGPM....................................................................................................... Conversion Factors.............................................................................................................................................................. Supplementary Metric Practice Guides ................................................................................................................................ : Bibliography Index 1 2 2.1 2.2 2.3 2.4 2.5 3 3.1 3.2 3.3 3.4 3.5 4 4.1 4.2 4.3 4.4 4.5 4.6 5 XI X2X3 X4 1. Scope 1.1 This standard gives guidance for application of The International System of Units (the modernized metric system) developed and maintained by the General Confer ence on Weights and Measures (abbreviated CGPM from the official French name Conference Generate des Poids et Mesures). The name International System of Units and the international abbreviation SI2 were adopted by the 11th CGPM in 1960. 1.2 Information is included on SI, a limited list of non-SI units recognized for use with SI units, and a list of conver sion factors from non-SI to SI units, together with generalguidance on proper style and usage. 1.3 It is hoped that an understanding of the system and its characteristics, and careful use according to this standard, 1 This standard is under the jurisdiction of ASTM Committee E-43 on Metric Practice and is the direct responsibility of Subcommittee E43.10 on Standards. Current edition approved Oct. 3, 1991. Published December 1991. Originally published in 1964 without designation as ASTM Metric Practice Guide, revised 1966. Adopted as standard 1968. Last previous edition E 380 - 89. 2 From the French name, Lc Systeme International d'Unites. will help to avoid the degradation that has occurred in all older measurement systems. 2. SI Units and Symbols__ 2.1 Classes of Units--SI units are divided into three classes: base units supplementary units derived units 2.2 Base Units--SI is based on seven well-defined units (see Table 1) which by convention are regarded as dimen sionally independent. 2.3 Supplementary Units--This class contains two units, the radian and the steradian (see Table 2). At the time of the introduction of the International System, the 11th CGPM left open the question of the nature of these supplementary units. Considering that plane angle is generally expressed as the ratio between two lengths and solid angle as the ratio between an area and the square of length, the CIPM (1980) specified that in the International System the quantities plane angle and solid angle should be considered as dimen- 1107 DUP050298284 E 380 TABLE 1 Base SI Units Quantity3 Unit length mass time electric current thermodynamic temperature'' amount of substance luminous intensity metre kilogram second ampere kelvln mole candela A For a discussion of Celsius temperature see 3.4.2. Symbol m *9 s A K mol cd TABLE 2 Quantity3 plane angle solid angle Supplementary SI Units Unit radian steradian Symbol rad sr sionless derived quantities. Therefore, the supplementary units radian and steradian are to be regarded as dimension less derived units which may be used or omitted in the expressions for derived units. 2.4 Derived Units: 2.4.1 Derived units are formed by combining base units, supplementary units, and other derived units according to the algebraic relations linking the corresponding quantities. The symbols for derived units are obtained by means of the mathematical signs for multiplication, division, and use of exponents. For example, the SI unit for velocity is the metre per second (m/s or m s-1), and that for angular velocity is the radian per second (rad/s or rad-s_!). 2.4.2 Those derived SI units which have special names and symbols approved by the CGFM are listed in Table 3. 2.4.3 It is frequently advantageous to express derived units in terms of other derived units with special names; for example, the SI unit for electric dipole moment is usually expressed as C-m instead of A-s-m. 2.4.4 Some common derived units are listed in Table 4. 2.5 SI Prefixes (see 3.2 for application): 2.5.1 The prefixes and symbols listed in Table 5 are used to form names and symbols of the decimal multiples and submultiples of the SI units except for kilogram. 2.5.2 Unit ofMass--Among the base and derived units of SI, the unit of mass (kilogram) is the only one whose name, for historical reasons, contains a prefix. Names of decimal multiples and submultiples of the unit of mass are formed by attaching prefixes to the word gram (g). 2.5.3 These prefixes or their symbols are directly attached to names or symbols of units, forming multiples and submultiples of the units. In strict terms these must be called "multiples and submultiples of SI units," particularly in discussing the coherence of the system (see Section 5). In common parlance, the base units and derived units, along with their multiples and submultiples, are all called SI units. 3. Application of the Metric System 3.1 General--SI is the form of the metric system that is preferred for all applications. It is important that this modernized form of the metric system be thoroughly under- 3 ''Quantity" as used in the headings of the tables of this standard means measurable attribute of phenomena or matter. TABLE 3 Derived SI Units with Special Names Quantity3 frequency {of a periodic phenomenon) force pressure, stress energy, work, quantity of heat power, radiant flux quantity of electricity, electric charge electric potential, potential difference, electromotive force electric capacitance electric resistance electric conductance magnetic flux magnetic flux density Unit hertz newton pascal jouie watt couiomb volt farad ohm siemens weber tesla Symbol Hz N Pa J W C V F ft s m T Fomiui! . ^bsorbeddosj 1/s acceleration }, kg-m/ss iHt H!m> N-m III angular aoceii angular vetocj area ] concentratioi. current dens > /s A-s m II density, mas. electric char W/A * electric field: electric flux Hi' energy den: c/v V/A A/V W entropy exposure 0 qeatcapac _ V-s H heat flux d Wb/m2 Ijff irradiattce inductance henry H Wb/A ft Celsius temperature degree C Kfsee 3-4.2 luminance CelsiusA magnetic! luminous flux illuminance lumen lux )m cd*sr .11 molar ens lx lm/m2 it molar erst] activity (of a radionuelid^ absorbed dose bfecquerel gray Bq V H molar hes' Gy 4/kg If momenft dose equivalent sievert Sv JAs * permeant A Inclusion In the table of derived SI units with special names approved by| CIPM In 1976. Related quantities using the same unit are: specific energy imparted, ki and absorbed dose index. permittiv] power di radiandej, radiant it; specific] specific it stood and properly applied. Obsolete metric units ai practices are widespread, particularly in those countries long ago adopted the metric system, and much usage suffapel thermal improper. This section gives guidance concerning the limit? number of cases in which units outside SI are appropriate! used, and makes recommendations concerning usage an| style. velocity viscqs] viscosf volurri^ . wave]., 3.2 Application ofSI Prefixes: i 3.4.4. j, 3.2.1 General--In general the SI prefixes (2.5) should b| used to indicate orders of magnitude, thus elirmnatinf .surementS i nonsignificant digits and leading zeros in decimal fractions .2.3 Prffigc and providing a convenient alternative to the powers-of-ter i only one .. notation preferred in computation. For example: .pound umt 12 300 mm becomes 12.3 m in the .nvf;. 12.3 X 103 m becomes 12.3 km 0.00123 pA becomes 1.23 nA igram dccu ? |amplesi 3.2.2 Selection--When expressing a quantity by a numer ical value and a unit, a prefix should preferably be chosen soj that the numerical value lies between 0.1 and 1000. To! 3,2.4 Comp. minimize variety, it is recommended that prefixes repre \ the juxtapjii, senting 1000 raised to an integral power be used. However, ed. For exajy three factors may justify deviation from the above: 3.2.2.1 In expressing area and volume, the prefixes hecto-, deka-, deci-, and centi- may be required, for example, square j values arjL; hectometre, cubic centimetre. 3.2.2.2 In tables of values of the same quantity, or in a discussion of such values within a given context, it is generally preferable to use the same unit multiple through out. 3.2.2.3 For certain quantities in particular applications, one particular multiple is customarily used. For example, the lefixes, the|,. jbplied to # t 3.2.5 Po% containing %. |f the unit ft ^pressed bfr, millimetre is used for linear dimensions in mechanical engineering drawings even when the values lie far outside the 4 A compoif^' range 0.1 to 1000 mm; the centimetre is often used for body knits rather th|r" 1108 IS/ DUP050298285 f # E 380 TABLE 4 Some Common Derived Units of SI \ Quantity3 Unit absorbed dose rate acceleration angular acceleration angular velocity area concentration (of amount of substance) current density density, mass electric charge density electric field strength electric flux density energy density entropy exposure (X and gamma rays) heat capacity gray per second metre per second squared radian per second squared radian per second square metre mole per cubic metre ampere per square metre kilogram per cubic metre coulomb per cubic metre volt per metre coulomb per square metre ., joule per cube metre joule per kelvin coulomb per kilogram joule per Kelvin Symbol Gy/s m/s2 rad/s2 rad/s m2 mol/m3 A/m2 kg/m3 C/m3 V/m C/m2 J/m3 J/K C/kg J/K heat flux density j Irradiance j watt per square metre W/mz 1 the ! ma, ixd mt is ed ly id luminance magnetic field strength - molar energy molar ontropy molar heat capacity moment of force* permeability {magnetic) permittivity power density radiance radiant intensity specific heat capacity specific energy specific entropy specific volume surface tension thermal conductivity velocity viscosity, dynamic viscosity, kinematic volume wave number candela per square metre ampere per metre joule per mole joule per mole kelvin joule per mole kelvin newton metre henry per metre farad per metre watt per square metre watt per square metre steradian watt per steradian joule per kilogram kelvin joule per kilogram joule per kilogram kelvin cubic metre per kilogram newton per metre watt per metre kelvin metre per second pascal second square metre per second cubic metre 1 per metre . - c.d/tn2 A/m J/mol J/jmol-K) J/(mol-K) N-m H/m F/m W/m2 W/(mz-sr) W/sr J/(kg-K) . J/kg J/(kg-K) m3/kg N/m W/(m-K) m/s Pa-s m2/s m3 1/m * See 3.4.4. ie fg iS, [measurements and clothing sizes. ! 3.2.3 Prefixes in Compound Units4--It is recommended that only one prefix be used in forming a multiple of a compound unit. Normally the prefix should be attached to a unit in the numerator. One exception to this is when the [kilogram occurs in the denominator. Examples: ro .V/m, not mV/mm, and MJ/kg, not kJ/g 0 3.2.4Compound Prefixes--Compound prefixes, formed 'by the juxtaposition of two or more SI prefixes are not to be [used. For example, use 1 nm, not 1 mpm I pF, not 1 (ipF I lf values are required outside the range covered by the prefixes, they should be expressed by using powers of ten i applied to the base unit. j 3.2.5 Powers of Units--An exponent attached to a symbol : containing a prefix indicates that the multiple or submultiple {of the unit (the unit with its prefix) is raised to the power [ expressed by the exponent. For example: 4 A compound unit is a derived unit that is expressed in terms of two or more units rather than by a single special name. l.cm3 = (10 2 m)3 1 ns"1 =(10-9s>-1 I mm2/s = (10~3 m)~/s = 10~6 m3 = 109 s-1 = 1(T6 m2/s 3.2.6 Calculations--Errors in calculations can be mini mized if the base and the coherent derived SI units are"used and the resulting numerical values are expressed in powersof-ten notation instead of using prefixes. 3.3Other Units: 3.3.1 Units from Different Systems--To assist in pre serving the advantage of SI as a coherent system, it is advisable to minimize the use with it of units from other systems. Such use should be limited to units listed in this section. 3.3.2 Units in Use with SI (see Table 6): 3.3.2.1 Time--The SI unit oftime is the second. This unit is preferred and should be used if practical, particularly when technical calculations are involved. In cases where time relates to life customs or calendar cycles, the minute, hour, day, and other calendar units may be necessary. For ex ample, vehicle speed will normally be expressed in kilometres per hour. 3.3.2.2 Plane Angle--The SI unit for plane angle is the radian. Use of the degree and its decimal submultiples is permissible when the radian is not a convenient unit. Use of 1109 DUP050298286 # E 380 TABLE 5 Si Prefixes Multiplication Factor Prefix 1 000 000 000 000 000 000 = 10'8 1 000 000 000 000 000-10'5 1 000 Q00 000 000 = 10'3 i ooo aoQ ooo = ia9 1 000 000- 10" : 1 000= 103 100= 102 10= 10' 0.1 = 10"' 0.01 = 10"2 0.001 = 10~3 0.000 001 = 10~6 0.000 000 001 = 10-9 0.000 000 000 001 = 10-'9 0.000 000 000 000 001 = 10-'5 0.000 000 000 000 000 001 = 10*'9 exa peta tera giga mega kilo hecto'' deka" deci* cent!" milli micro nano pico femto atto A To tie avoided where practical, except as noted in 3,2.2. Symbol E P T G M k h da d c m n p f a the minute and second is discouraged except for special fields such as, cartography. 3.3.X3 Area--The SI unit of area is the square metre (m2). The hectare (ha) is a special name for square hectometre (hm2). Large land or water areas are generally expressed in hectares or in square kilometres (km2). 3.3.2.4 Volume--The SI unit of volume is the cubic metre. This unit, or one of the regularly formed multiples such as the cubic centimetre, is preferred. The special name litre' (L)6 has been approved for the cubic decimetre, but use of this unit is restricted to volumetric capacity, dry measure,, and measure of fluids (both gases and liquids). No prefix other than milli- or micro- should be used with litre. 3.3.2.5 Mass--The SI unit of mass is the kilograrn. This unit, or one of the multiples formed by attaching an SI prefix to gram (g), is preferred for all applications. The megagram (Mg) is the appropriate unit for measuring large masses such as have been expressed in tons. However, the name ton has been given to several large mass units that are widely used in commerce and technology--the long ton of 2240 lb, the short ton of 2000 lb, and metric ton of 1000 kg (also called the tonne). None of these terms are SI. The term metric ton should be restricted to commercial usage, and no prefixes should be used with it. Use of the term tonne is deprecated. 5 See Appendix XI. 11.1. ! 6 The CCJPM in October 1979 approved L and I as alternative symbols for litre. Since the letter symbol 1 can easily be confused with the numeral 1, only the symbol L is recommended for USA use. TABLE 6 Units in Use with SI Quantity3 time plane angle Unit minute hour day week, month, etc. degree minute'" second'4 volume mass area Hire metric ton hectare Symbol min h d 0 L t ha 1 min 1h 1d Definition 1= 60s a 60 min = 3600 s 88 24h = 86 400s 1 = pr/180) rad V * (1/60) (ir/10 800) rad 1" (1/60)' S- fr/648 000) rad 1 L S= 1 dm3 * 10~3 m3 1 t = 103 kg 1 ha = 1 hm2 104 m2 A Use discouraged except for special fields such as cartography. s See 3.3.2.4. 3.3.3 Units in Use with SI Temporarily (see Table 7); 3.3.3.1 Energy--The SI unit of energy, the joule, together with its multiples, is preferred for all applications. The kilowatthour is widely used, however, as a measure of electric energy. This unit should not be introduced into any new areas, and eventually it should be replaced by the megajoule. 3.3.3.2 Pressure and Stress--The SI unit of pressure and stress is the pascal (newton per square metre) and with proper SI prefixes is applicable to all such measurements. Old metric gravitational units for pressure and stress such as kilogram-force per square centimetre (kgf/cm2) shall not be used. Widespread use has been made of other* non-SI units such as bar and torr for pressure, but this use is strongly discouraged. The millibar is widely used in meteorology; this usage will continue for the present in order to permit meteorologists to communicate easily within their profes sion. The kilopascal should be used in presenting meteoro logical data to the public. 3.3.4 Units and Names to Be Abandoned--A great many metric units other than those of the SI have been defined over the years. Some of these are used only in special fields; others have found broad application in countries that adopted the metric system early. Except for the special cases discussed in the previous sections, non-SI units (as well as special names for multiples or submultiples of SI units) are to be avoided. Various categories of deprecated units are discussed in 3.3.4.1 to 3.3AA. The lists are not intended to be complete, but only to indicate more or less prominent examples of each category. 3.3.4.1 Cgs Units--All units peculiar to the various cgs systems (measurement systems constructed by using the centimetre, gram, and second as base units) are to be avoided. Among these units are the following, defined for mechanics, fluid mechanics, and photometry, the erg, dyne, gal, poise, stokes, stilb, phot, and lambert. Further use of the cgs units of electricity and magnetism is deprecated. This statement applies to the units designated by the general abbreviations "esu" (for electrostatic cgs unit) and "emu" (for electromagnetic cgs unit), including those units that have been given special names--the gauss, oersted, maxwell, gilbert, biot, and franklin. It also applies to the unit names formed with the prefixes.-ab- and `Stat-, for example, the abampere, statvolt, etc. 3.3.4.2 Decimal Multiples of SI Units--Those multiples of SI units that cannot be handled by using the SI prefixes are deprecated. Many such examples are covered in subsection 3.3.4.1. An additional example is the angstrom (0.1 nm). 3.3.4.3 Unit Names to Be Avoided--Special names for TABLE 7 Units in Use with SI Temporarily Quantity3 Unit Symbol Definition energy [see 3.3.3.1] cross section pressure [see 3.3.3.2J activity (of a radio- nuclide) exposure (X and gamma rays) absorbed dose dose equivalent kilowatthour bam bar curie roentgen rad rem kWh b bar Ci R rd rem 1 kWh 3.6 MJ 1 b =r 10-"m2 = 100 fm2 1 bar 10s Pa 1 Ci 3.7 x 10' Bq 1 R - 2.58 x ur4 C/kg 1 rd as 0.01 Gy 1 rem 0.01 Sv = 10 mSv mo idej 1 fi. 'U j;:r. (`A DUP050298287 : and with ents. chas at be units rngly ; this rmit ofes:oro- 380 aultiples and submultiples of SI units are to be avoided jjbxcept for the litre (3.3.2.4), metric ton (3.3.2.5), and hectare |3.3.2.3). For example, do not use: E 7o II s. II Jtermi.............................. 1 fermi feiicron.......................... 1 micron millimicron................... 1 millimicron fare................................ 1 are pamma.......................... 1 gamma b (magnetic flux density) Iy (mass)........................ 1 7 Ik (volume)..................... 1 X femho.............................. 1 mho [candle............................ 1 candle jicandlepower................... 1 candlepower = 1 pm = 10~6 m = 1 nm = 10~9 m = 1 dam2 = 100 m: = 1 nT = 1 ug = 1 pL = 1 mm3 =1S = ! cd = 1 cd 3.3.4.4 Miscellaneous Units--Other non-SI units that are i deprecated include the following: calorie grade [1 grade = (ir/200) rad] , kilogram-force - langley (= 1 cal/cm2) metric carat metric horsepower millimetre of mercury millimetre, centimetre, metre of water standard atmosphere (1 atm = 101.325 kPa) technical atmosphere (1 at = 98.0665 kPa) torr 3.4 Other Recommendations Concerning Units: 3.4.1 Mass, Force, and Weight: 3.4.1.1 The principal departure of SI from the gravimetric system of metric engineering units is the use of explicitly distinct units for mass and force. In SI, the name kilogram is restricted to the unit of mass, and the kilogram-force (from which the suffix force was "in practice often erroneously dropped) should not be used. In its place the SI unit of force, the newton, is used (see Fig. 1). Likewise, the newton rather than the kilogram-force isused to form derived units which include force, for example, pressure or stress (N/m2 = Pa), energy (N m = J), and power (N m/s = W). 3.4.1.2 Considerable confusion exists in the use of the term weight as a quantity to mean either force or mass. In commercial and everyday use, the term weight nearly always means mass; thus, when one speaks of a person's weight, the quantity referred to is mass. This nontechnical use of the term weight in everyday life will probably persist. In science and technology, the term weight ofa body has usually meant les ire on mass 1 kg Moon mass i 1kg i Earth FIG. 1 Illustration of Difference Between Mass (Unit = kilogram = kg) and Force (Unit = newton = N) (see 3.4.1) 1111 |i.., I I DUP050298288 E 380 the force that, if applied to the body, would give it an acceleration equal to the local acceleration of free fall. The adjective "local" in the phrase "local acceleration of free fall" has usually meant a location on the surface of the earth; in this context the "local acceleration of free fall" has the symbol g (commonly referred to as "acceleration of gravity") with observed values of g differing by over 0.5 % at various points on the earth's surface. The use offorce ofgravity (mass times acceleration of gravity) instead of weight with this meaning is recommended. Because of the dual use of the term weight as a quantity, this term should be avoided in technical practice except under circumstances in which its meaning is completely clear. When the term is used, it is important to know whether mass or force is intended and to use SI units properly as described in 3.4.1.1, by using kilograms for mass or newtons for force. 3.4.1.3 Gravity is involved in determining mass with a balance or scale. When a standard mass is used to balance the measured mass, the effects of gravity on the two masses are equalized, but the effects, of the buoyancy of air. or other fluid on the two masses are generally not equalized. When a spring scale is used, the scale reading is directly related to the force of gravity. Spring scales graduated in mass units may be properly used if both the variation in acceleration of gravity and the buoyancy corrections are not significant in their use. 3.4.1.4 The use of the same name for units of force and mass causes confusion. When the non-SI units are used, a distinction should be made between force and mass, for example, Ibf to denote force in gravimetric engineering units and lb for mass. 3.4.1.5 The term load means either mass or force, de pending on its use. A load that produces a vertically downward force because of the influence of gravity acting on a mass may be expressed in mass units. Any other load is expressed in force units. 3.4.2 Temperature--The SI unit of thermodynamic tem perature is the kelvin (K), and this unit is properly used for expressing thermodynamic temperature and temperature intervals. Wide use is also made of the degree Celsius (C), which js the SI unit used for expressing Celsius temperature and temperature intervals. The Celsius scale (formerly called centigrade) is related directly to thermodynamic temperature (kelvins) as follows: The temperature interval one degree Celsius equals one kelvin exactly. Celsius temperature (t) is related to thermodynamic tem perature (7) by the equation: t=T-T0 where T0 = 273.15 K by definition. The International Practical Temperature Scale (IPTS) must be recognized in temperature work of extreme precision. See ASTM STP 565, Evolution of the International Practical Temperature Scale of 1968. 3.4.3 Linear Dimensions: 3.4.3.1 Nominal dimensions name the item; no SI equiv alent is required (see Section 5 for definition of "nominal value"). For example, there is nothing "I in" about a nominal "1-in pipe," the dimensions of which should be converted as follows: Nominal Size, inches 1 Outside Diameter, inches (mm) 1.315 (33.40) Wall Thickness, inches (rani) Sch 40 Sch 80 Sch 160 0.133 (3.38) 0.179 (4.55) 0.250 (6.35) Likewise, a "2 by 4" is that in name only and refers to , approximate dimensions in inches of a rough-sawn piece' green lumber, the finished dimensions of which are ( (G_ 5.4.7.1 T jr exam pressed t sunit is ;ssed I 1.4.7.2 per r 1.4.7.3 erably less. A `/4-20 UNC screw thread should continue to ressioi identified in this manner. However, the controlling dimei sions of the part, such as .the pitch, major, and mini , 1.2 p: sampl diameters of a screw thread, should be converted to SI valu< in accordance with 4.1 and 4.2. juld no jresstoi 3.4.3.2Surface texture should be expressed in microi sent. etres. (3.5 Sty 3.4.4 Quantities and Units used in Rotational Mechank lbols 3.4.4.1 Angle, Angular Velocity, andAngular Acceleratioi Their SI units are rad, rad/s, and rad/s2 respectively. L accordance with Sec. 2.3, since the radian is here taken to dimensionless, the units-1, 1/s, and 1/s2 are also used whei appropriate. 3.4.4.2 Moment ofForce (Torque or Bending Moment) isi liform iguage; iprove 3.5.1 3.5. ill force times moment arm (lever arm). Its SI unit is N m. ardles 3.4.4.3 Moment of Inertia (/) is a property of the mass; 3.5.11 distribution of a body about an axis (7 = 'Zmr2), Its SI unit is 3.5.U: kg- m2. vhen us 3.4.4.4 Angular Momentum (moment of momentum) is 3.5.1.' linear momentum (kg-m/s) times moment arm (m). Its SI unit is kg-m2/s. For a rotating body the total angular momentum is equal to the moment of inertia I (kg-m2) oper; .pitalii times the angular velocity 9 (rad/s or 1 /s). mbolj 3.4.4.5 Rotational Kinetic Energy of a rotating body is ipper-ct equal to 'A/9 2. Its SI unit is J. resciit|, 3.4.4.6 Rotational Work is equal to torque (N nr) times 'or syij angle of rotation (rad). Its SI unit is J. efer fcoj' 3.4.4.7 Torsional Stiffness (torsion constant) of a body is symbol applied torque (N-m) divided by angle of twist (rad). Its SI fieidpi unit is N m/rad. missibj 3.4.4.8 Centripetal Acceleration, v2jr or 2r, where v is the symbo|- tangential linear velocity (m/s), r the radius (m), and w.the angular velocity (rad/s) is, like any other linear acceleration, measured in SI units m/s2. those tf betwee sets .nj|;v N)*' --Centripetal Force, equal to mass times centripetal accelera tion, is, like any force in SI, measured in newtons. permi ~ this stv 3.4.5 Impact Energy Absorption--This quantity, often incorrectly called impact resistance or impact strength, is measured in terms of the work required to break a standard specimen; the proper unit is joule. 3.4.6 Pressure and Vacuum--Gage pressure is absolute pressure minus ambient pressure (usually atmospheric pres sure). Both gage pressure and absolute pressure are properly expressed in pascals, using SI prefixes as appropriate. Abso lute pressure is never negative. Gage pressure is positive if above ambient pressure and negative if below. Pressure below ambient is often called vacuum; whenever the term vacuum is applied to a numerical measure it should be made clear whether negative gage pressure or absolute pressure is meant. See 3.5.5 for methods of designating gage pressure and absolute pressure. 3.4.7 Dimensionless Quantities: and ary examjfJ lumex! ! Ext j and 1 anglUyL 3-fy is usp; instep betv|j 1112 DUP050298289 # E 380 if 3.4.7.1 The values of so-called dimensionless quantities, for example refractive index and relative permeability, are expressed by pure numbers. In these cases the corresponding H unit is the ratio of the same two SI units and may be Expressed by the number 1. tilt! 1 3.4.7.2 Terms such as percent, parts per thousand, and e of Jarts per million may also be used. fuel-, 3.4.7.3 In all cases, the meaning must be unequivocal. 3 be Expressions like "The mole fraction of C02 in the sample icn- Sms 1.2 parts per million" or "The mass fraction of C02 in cor lie sample was 1.2 parts per million" are permissible, but UC& would not be permissible if the word "mole" in the first Ixpression or "mass" in the second expression were not )in- Sresent. * 3.5 Style and Usage--Care must be taken to use unit zci. |ymbols properly, and international agreement provides on. iform rules. Handling of unit names varies because of In anguage differences, but use of the rules included here will be bnprove communications in the United States. ion 3.5.1 Rules for Writing Unit Symbols: ) ih 3.5.1.1 Unit .symbols should be printed in upright type Regardless of the type style used in the surrounding text. 3SN 3.5.! .2 Unit symbols are unaltered in the plural. is 3.5.1.3 Unit symbols are not followed by a period except rhen used at the end of a sentence. is 3.5.1.4 Letter unit symbols are written in lower-case (for SI ixample, cd) unless the unit name has been derived from a lai roper name, in which case the first letter of the symbol is i2) apitalized (for example, W, Pa). The exception is the Symbol for litre, L. Prefix symbols use either lower-case or pper-case letters as shown in 2.5.1. Symbols retain their prescribed form regardless of the surrounding typography. es "or symbols for use in systems with limited character sets, refer to ANSI X3.50 or ANSI/IEEE 260, as applicable. The 15 symbols in ANSI X3.50 are intended for applications in the SI' field of information processing, where unambiguous trans mission of information between computers is required. The [symbols in ANSI/IEEE 260 are generally consistent with those in ANSI X3.50 and are intended for communication between human beings. The symbols for limited character (sets must ..never be used when the available character set [permits the use of the proper general-use symbols as given in ithis standard. 3.5.1.5 When a quantity is expressed as a numerical value nd a unit symbol, a space should be left between them. For (example, use 35 mm, not 35mm, and 2.37 1m (for 2.37 [lumens), not 2.371m. Exception: No space is left between the numerical value and the symbols for degree, minute, and second of plane angle, and degree Celsius. For example, use 45, 20C. 3.5.1.6 When a quantity expressed as a number and a unit is used in an adjectival sense, it is preferable to use a hyphen instead of a space between the number and the unit name or between the number and the symbol. Examples: A three- metre pole. .. The length is 3 m. .. A 35-mm film... The width is 35 mm. However, per 3.5.1.5 Exception, a 90 angle... an angle of 90. 3.5.1.7 No space is used between the prefix and unit symbols. 3.5.1.8 Symbols, not abbreviations, should be used for units. For example, use "A" and not "amp" for ampere. 3.5.2 Rules for Writing Names: 3.5.2.1 Spelled-out unit names are treated as common nouns in English. Thus, the first letter of a unit name is not capitalized except at the beginning of a sentence or in capitalized material such as a title. 3.5.2.2 Plurals are used when required by the rules of English grammar and are normally formed regularly, for example, henries for the plural of henry. The following irregular plurals are recommended: Singular ' Plural lux hertz siemens lux hertz siemens 3.5.2.3 No space or hyphen is used between the prefix and unit name. There are three cases where the final vowel in the prefix is commonly omitted: megohm, kilokfn, and hectare. In all other cases where the .unit name begins with a vowel both vowels are retained and both are pronounced. 3.5.3 Units Formed by Multiplication and Division: 3.5.3.1 With unit names: Product, use a space (preferred) or hyphen: newton metre or newton-metre In the case of the watt hour the space may be omitted, thus: watthour Quotient, use the word per and not a solidus: metre per second, not metre/second Powers, use the modifier squared or cubed placed after the unit name: metre per second squared In the case of area or volume, the modifier may be placed before the unit name: square millimetre, cubic metre This alternative is also allowed for derived units that include area or volume: watt per square metre N+,' --To avoid ambiguity in complicated expressions, symbols are preferred over words. 3.5.3.2 With unit symbols: Product, use a raised dot: N m for newton metre In the case of W-h, the dot may be omitted, thus: Wh An exception to this practice is made for computer print outs, automatic typewriter work, etc., where the raised dot is not possible, and a dot on the line may be used. Quotient, use one of the following forms: m/,s or m-s-l' or --ui In no case should more than one solidus be used in the same 1113 DUP050298290 E 380 expression unless parentheses are inserted to avoid ambi guity. For example, write: J/(mo! K) or J mol~1 K~' or (J/mol)/K, but not J/mol/K 3.5.33 Symbols and unit names should not be mixed in the same expression. Write: joules per kilogram or J/kg or J - kg"' but not joules/kilogram nor joules/kg nor joules-kg-1 3.5.4 Numbers: 3.5.4.1 The recommended decimal marker is a dot on the line. When writing numbers less than one, a zero should be written before the decimal marker. 3.5.4.2 Outside the United States, the comma is often used as a decimal marker. In some applications, therefore, the common practice in the United States of using the comma to separate digits into groups of three (as in 23,478) may cause ambiguity. To avoid this potential source of confusion, recommended international practice calls for separating the digits into groups of three, counting from the decimal point toward the left and the right, and using a small space to separate the groups. In numbers of four digits on either side of the decimal point the space is usually not necessary, except for uniformity in tables. Examples: ' 2.141 596 73 722 7372 0.1335 Where this practice is followed, the space should be narrow (approximately the width of the letter "i"), and the width of the space should be constant even if, as is often the case in printing, variable-width spacing is used between words. Exceptions: In certain specialized applications, such as engineering drawings and financial statements, the practice of using a space for a separator is not customary. 3.5.4.3 Because billion means a thousand million (prefix giga) in the United Slates but a million million (prefix tern) in most other countries, this term and others, such as trillion, should be avoided in technical writing. 3.5.4.4 Use of M to indicate thousands, as in MCF for thousands of cubic feet, or in MCM for.thousands of circular mils, of MM to indicate millions, of C to indicate hundreds, etc., is deprecated because of obvious conflicts with the SI prefixes. 3.5.5 Attachment--Attachment of letters to a unit symbol as a means of giving information about the nature of the quantity under consideration is incorrect. Thus MWe for "megawatts electrical (power)," Vac for "volts ac,'' and kJt for "kilojoules thermal (energy)" are not acceptable. For this reason, no attempt should be made to construct SI equiva lents of the abbreviations "psia" and "psig," so often used to distinguish between absolute and gage pressure. If the context leaves any doubt as to which is meant, the word pressure must be qualified appropriately. For example: ".,. at a gage pressure of 13 kPa" or "., . at an absolute pressure of 13 kPa" Where space is limited, such as on gages, nameplates, graph labels, and in table headings, it is permissible to use the unit symbol followed by a space and the modifier in parentheses For example: V (ac) and V (die); kPa (gage) and kPa (absolute). 3.5.6 Pronunciation-Some recommended pronuncia tions in English are shown in Table 8. 4. Rules for-Conversion and Rounding 4.1 General: 4.1.1 Conversion factors to change a value of a quantity expressed in non-SI units to the corresponding value of that quantity expressed in the International System of Units may be exact or approximations adequate for the particular task. The rules in this section are based on using either exact or approximate factors such as those of seven-digit factors listed in Appendix X3. In some cases the quantity is such that factors with fewer digits are appropriate. 4.1.2 Conversion of quantities should be handled:with careful regard to tfie implied correspondence between the accuracy of the data and the given number of digits. In all conversions, the number of significant digits retained should be such that accuracy is neither sacrificed nor exaggerated. (For guidance concerning significant digits see 4.3.) For example, a length of 125 ft converts exactly to 38.1 m. If, however, the 125-ft length had been obtained by rounding to the nearest 5 ft, the conversion should be given as 38 m; and if it had been obtained by rounding to the nearest 25 ft, the conversion should be given as 40 m. 4.1.3 Proper conversion procedure is to multiply a value by a conversion factor that is more accurate than is required; the result is then rounded to the appropriate number of sig nificant digits. For example, to convert 3 feet 29/is inches to metres: (3 x 0.3048) + (2.5625 x 0.0254) = 0.979 487 5 m,' which rounds to 0.979 m. Do not round either the conver sion factor or the quantity before performing the multiplica tion, as accuracy may be reduced. After the conversion, the TABLE $ Recommended Pronunciation _______ Prefix____________________ Pronunciation (USA)"* exa.........................................................ex'a (a as in about) peta.......................................................pet' a (e as in pel, s as in about) tera ...................................................--as in terra firms giga.......................................................jig' a (/ as in j/g, a as in about) mega.................................................... as in megaphone Kilo.........................................................kilT oh hecto..............................!.....................heck' toe deka........ ................. .........................deck' a (a as in about) dec!............. ...................................... as in decimal centi.......................................................as in centipede milii.............................................. .... as in military micro.................................................... as in microphone nano.......................................................nan' oh (an as in ant) pico...................................................... peek' oh femto.................................................... fern' toe (fem as in feminine) atto.................................................. .as in anatomy Selected Units Pronunciation candela.................................................. can tfe//' a jouie.......................................................rhyme with tool kilometre................................................ kid ' oh metra pascaf.................................................... rhyme with rascal siemens................................................ same as seamen's A The first syllable of every prefix is accented la assure that the prefix wifi retain its identity. Therefore, the preferred pronunciation of kilometre places the accent on the first syllable, not the second. 1114 :I valu I by t 4.2 lUltif: r,odu onve: signifii onve. ie or Ibonsic' visic' iineasu ibvioi or cal;: to on situatu propel! |Two <j tdsscrii 4.2 [first fquanrt: I retain, the q |A ftsv | nqncri ! the Qt : mean writte : intenc i estim: the ac thaii : the. jp; shonk ' digits small' DUP050298291 ;s, nameplates, graph issible to use the unit differ in parentheses. Pa (gage) and kPa (tended pronuncia- value of a quantity ending value of that ystem of Units may the particular task, sing either exact or n-digit factors listed antity is such that 1 be handled with ience between the ter of digits. In all its retained should i nor exaggerated, gits see 4.3.) For ttly to 38.1 m. If, ed by rounding to liven as 38 m; and nearest 25 ft, the multiply a value : than is required; te number ofsig:et 29/i6 inches to = 0.979 487 5 m, ither the converg the multiplica; conversion, the ation iatlon (USA)"4 iutji *, a as in about) J as in about) 30Ut) nt) i feminine) ciation he prefix will retain places the accent SI value may be expressed by a multiple or submultiple unit of SI by the use of an appropriate prefix, for example, 979 mm. 4.2 Accuracy and Rounding--A conversion obtained by multiplying a value by a seven-digit factor usually gives a product with more digits than the original value. The converted value must be rounded to the proper number of significant, digits commensurate with the intended accuracy. Conversions usually yield a product with more, digits than the original value. The practical aspect of measuring must be considered when using SI equivalents. If a scale having division of >/i6 inch was suitable for making the original measurements, a metric scale having divisions of 1 mm is obviously suitable for measuring in SI units, Similarly, a gage or caliper graduated in divisions of 0.02 mm is comparable to one graduated in divisions of 0.001 in. Analogous situations exist in mass, force, and other measurements. Many techniques are used to guide the determination of the proper number of significant digits in the converted values. Two different approaches tp rounding of quantities are here described-r-one for general use and the other for conversion of dimensions involving mechanical interchangeability. 4.2.1 General Conversion--This approach depends on first establishing the intended precision or accuracy of the quantity as a necessary guide to the number of digits to retain. This precision, should relate to the number of digits in the original, but in many cases this is not a reliable indicator. A figure 1.1875 may be a very accurate decimalization of a noncritical l3/i6 that should have been expressed 1.19. On the other hand, the value 2 may mean "about 2," or it may mean a very accurate value, of 2 which should have been written 2.0000. It is therefore necessary to determine the intended precision of a quantity before converting. This estimate of intended precision should never be smaller than the accuracy of measurement and should usually be smaller than one tenth the tolerance if one exists. After estimating the. precision of the dimension, the converted dimension should be rounded to a minimum number of significant digits (see 4.3) such that a unit of the last place is equal to or smaller than the converted precision. Examples: 1. A stirring rod 6 in. long. In this case, precision is estimated to be about 'h in ( `A in). Converted, this is 12.7 mm. The converted dimension 152.4 mm should be rounded to the nearest 10 mm, or 150 mm. 2. 50 000 lbf/in2 (psi-j tensile strength. In this case, precision is estimated, to be about 200 lbf/in2 ( 1.4 MPa) based on an accuracy of 0.25 % for the tensile tester and other factors. Therefore, the converted dimension, 344.7379 MPa, should be rounded to the nearest whole unit, 345,MPa. 3. Test pressure 200 15 lbf/in2 (psi). Since one tenth of the tolerance is 3 lbf/in2 (20.68 kPa), the converted dimen sion should be rounded to the nearest 10 kPa. Thus, 1378.9514 103.421 35 kPa becomes 1380 100 kPa. 4.2.2 Special Cases: 4.2.2,1 Converted values should be rounded to the min imum number of significant digits that will maintain the required accuracy, as discussed in 4.1.2. In certain cases deviation from this practice to make use of convenient or whole numbers may be feasible, in which case the word "approximate" must be used following the conversion. For example: l'/a ia = 47.62$ nrm^exact 47.6 mm .normal rounding s 47.5 mm (approx) rcsunded to preferred nu|| 48 mm (approx) rounded to whole number! 4.2.2.2 A quantity stated as a limit, such as than" or "maximum," must be handled so that f limit is not violated. For example, a specimen "all wide" requires a width of at least 101.6 mm, or atf mm. ` 4.3 Significant Digits: 4.3.1 When converting integral values of units, i ation must be given to the implied or required pr|| the integral value to he converted. For example, the in" may be intended to represent 4, 4.0, 4.00, 4.0000 in, or even greater accuracy. Obviously, the t value must be carried to a sufficient number off maintain the accuracy implied or required in the quantity. 4.3.2 Any digit that is necessary to define the) value or quantity is said to be significant. When mea the nearest 1 m, a distance may be recorded as 15*1 number has three significant digits. If the measuren been made to the nearest 0.1 m, the distance may Mi 157.4 m; this number has four significant digits. 4.3.3 Zeros may be used either to indicate a specif like any other digit, or to indicate the order of magnf a number. The 1970 United States population!, rounded to thousands was 203 185 000. The six lri digits of this number are significant; each measure's \ The three right-hand digits are zeros which merely ' the order of magnitude of the number rounded to the' thousand. The identification of significant digits possible through knowledge of the circumstances, t ample, the number 1000 may be-rounded from " which case only one zero is significant, or it may be i. from 999.7, in which case all three zeros are signifid 4.3.4 Occasionally data required for an investigate be drawn from a variety of sources where they ha recorded with varying degrees of. refinement. Specif, must be> observed when such data ate to. be addif- traded, multiplied, or divided..__ .. 4.3.4.1 The rule for addition and subtraction is answer shall contain no significant digits farther to tlf' than occurs in the least precise number. Consic addition ofthree numbers drawn from three sources, jp < of which reported data in millions, the second in thof- and the third in units: 163 000 000 F 217 885 000 v 96 432 768 . f. 477 "3(7 768 jp The total indicates a precision that is not vali^'numbers should first be rounded to one significatf farther to the right than that of the least precise numt|; the sum taken as follows: 163 000 000 217 900 000 96 400 000 477 300 000 1115 DUP050298292 E 380 The total is then rounded to 477 000 000 as called for by the rule. Note that if the second of the figures to be added had been 217 985 000, the rounding before addition would have produced 218 000 000, in which case the 0 following 218 would have been a significant digit. 4.3.4.2 The rule for multiplication and division is that the product or quotient shall contain no more significant digits than are contained in the number with the fewest significant digits used in the multiplication or division. The difference between this rule and the rule for addition and subtraction should be noted; the latter rule merely requires rounding of digits that lie to the right of the last significant digit in the least precise number. The following illustration highlights this difference: Multiplication: 113.2 x 1.43 = 161.876, rounded to 162 Division: 113.2 + 1.43 - 79.16, rounded to 79.2 Addition.* 113.2 + 1.43 = 114.63, rounded to 114.6 Subtraction: 113.2 - 1.43 = 111.77, rounded to 111.8 The above product and quotient are limited to three signifi cant digits since 1.43 contains only three significant digits. In contrast, the rounded answers in the addition and subtrac tion examples contain four significant digits. 4.3.4.3 Numbers used in the above illustrations have all been estimates or measurements. Numbers that are exact counts are treated as though they consist of an infinite number of significant digits. More simply stated, when a count is used in computation with a measurement the number of significant digits in the answer is the same as the number of significant digits in the measurement. If a count of 40 is multiplied by a measurement of 10.2, the product is 408. However, if 40 were an estimate accurate only to the nearest 10, and hence contained but one significant digit, the product would be 400. 4.4 Rounding Values1-. 4.4.1 When a figure is to be rounded to fewer digits than the total number available, the procedure should be as follows: 4.4.2.1 When the first digit discarded is less than 5, the last digit retained should not be changed. For example, 3.463 25, if rounded to four digits, would be 3.463; if rounded to three digits, 3.46. 4.4.1.2 When the first digit discarded is greater than 5, or if it is a 5 followed by at least one digit other than 0, the last digit retained should be increased by one unit. For example 8.376 52, if rounded to four digits, would be 8.377; if rounded to three digits 8.38. 4.4.1.3 When the first digit discarded is exactly 5, followed only by zeros, the last digit retained should be rounded upward if it is an odd number, but no adjustment made if it is an even number. For example, 4.365, when rounded to three digits, becomes 4.36. The number 4.355 would also round to the same value, 4.36, if rounded to three digits. 4.5 Conversion of Linear Dimensions of Interchangeable Parts--The use of the exact relation 1 in = 25.4 mm generally produces converted values containing more dec imal places than are required for the desired accuracy. It is therefore necessary to round these values suitably and at the same time maintain the degree of accuracy in the converted values compatible with that of the original values. 4.5.1 General--The number-of decimal places given in Table 9 for rounding converted toleranced dimensions relates the degree of accuracy to the size of the tolerances specified. Two methods of using Table 9 are given: Method A, which rounds to values nearest to each limit, and Method B, which rounds to values always inside the limits. In Method A, rounding is effected to the nearest rounded value of the limit, so that, on the average, the convened; tolerances remain statistically identical with the original tolerances. The. limits converted by this method, where acceptable for interchangeability, serve as a basis for inspec tion. In Method B, rounding is done systematically toward the interior ofthe tolerance zone so that the converted tolerances are never larger than the original tolerances. This method must be employed when the original limits have to be respected absolutely, in particular, when components made to converted limits are to be inspected by means of origin af gages. Method A--The use of this method ensures that even in'.j the most unfavorable cases neither of the two original limits will be changed by more than 5 % of the value of the tolerance. Proceed as follows: (a) Calculate the maximum- and minimum limits in inches. (b) Convert the corresponding two values exactly inter! millimetres by means of the conversion factor 1 in = 25.4' mm. (c) Round the results obtained to the nearest rounded value as indicated in Table 9, depending on the original! tolerance in inches, that is, on the difference between the two limits in inches. ~ if - Method B--This method~must be employed when the original limits may not be violated, for instance, certain critical mating parts. In extreme cases, this method naa.jf increase the lower limit a maximum of 10 % of the tolerance' and decrease the upper limit a maximum of 10 % of th e tolerance. (a) Proceed as in Method A step (a). lb) Proceed as in Method A step (b). l c) Round each limit toward the interior of the tolerance, that is, to the next lower value for the upper limit and to the next higher value for the lower limit.8 Examples: 7 Adapted from ISO R37G (7). 8 Ifthe digits to be rounded are zeros, the retained digits remain unchanged. sqle rukr cqn evtjii wp post! ni6 {' 11,, DUP050298293 E380 unded to ould also digits. langeable 15.4 mm sore decacy. It is nd at the onverted A dimension is expressed in inches as................... 1.95& 0.016 I 1 The limits are ...... ......................................... j Conversion of the two limits into millimetres fi* gives ......................... i......................... Method A--The tolerance equals 0.032 in and 1.934 and 1.966 49.1236 land 49,9364 thus lies between 0.004 and 0.04 in .(see Table ; 9). Rounding these values to the nearest 0.01 mm, the values in millimetres to be employed . -. for these two limits are .............................. . 49.12 and 49.94 Method B--Rounding toward the .interior of the tolerance, millimetre' values tor these two '49A3 and 49.93 limits are......... .......................................... ' [This reduces the tolerance to 0.80 instead of 0.82 mm given by Method ft. given in tensions olerances Method Method 4.5.2 Special Methodfor Dimensions with Plus and Minus Deviations--In order.'ta avoid accumulation of rounding (errors, the two limits.of size normally are converted sepa rately: thus, they must.first'be calculated if the dimension consists of a basicsi^e and two deviations.- However (except rounded onverted original l, where f inspec- when Method B is specified) as an alternative, the basic size may be, converted..to the nearest rounded value and each of | the deviations converted.towurd the interior of the tolerance. | This method, which sometimes makes conversion easier* gives the same maximum guarantee of accuracy as Method A, but usually results in smaller converted tolerances. vard the iterances method e to be ts made original 4.5.3 Special Methods for Limitation Imposed by Accu\ racy ofMeasurements--If the increment of rounding lor the ; tolerances given in Table 9 is too small for the available accuracy of measurement, limits that are acceptable for interchangeability must be determined separately for the dimensions. For example, where accuracy of measurement is limited to 0.001 mm, study shows that values converted even in al limits of the from 1.0000 0.0005 in can be rounded to 25.413 and 25.387 mm instead of 25.4127 and 25.3873 mm with little disadvantage, since neither of the two original limits is exceeded by more than 1.2 % of the tolerance. mits in 4.5.4 Positional Tolerance--If the dimensioning consists solely of a positional tolerance around a point defined by a i nontoleranced basic dimension, the basic dimension must be tly into = 25.4 converted to the nearest rounded value and the positional variation (radius) separately converted by rounding down ounded original the two ward. 4.5.5 Toleranced Dimension Applied to a Nontoleranced Position Dimension--If the toleranced dimension is located ; in a plane, the position of which is given by nontoleranced ten the certain id may lerance of the basic- or gage dimension, such as when dimensioning certain conical surfaces, proceed as follows: ( ) Round the converted reference gage arbitrarily, to the nearest convenient value. ( ) Calculate exactly, in the converted unit of measure ment, new maximum and minimum limits of the specified tolerance zone, in the new plane defined by the new basic dimension. France, to the (c) Round these limits in conformity with the rules in 4.4. For example, a cone of taper 0.05 in/in has a diameter of 1.000 0.002 inch in a reference plane located by the nontoleranced dimension 0.9300 in. By virtue of the taper of the cone, the limits of the tolerance zone depend on the position of the reference plane. Consequently, if the dimen .anged. sion 0.9300 in = 23.6220 mm is rounded to 23.600 mm (that is, a reduction of 0.022 mm), each of the two original limits, when converted exactly into millimetres, must be corrected by 0.022 x 0.05 = 0.0011 mm, in the appropriate sense, before being rounded. 4.5.6 Consideration ofMaximum and Minimum Material Condition--The ability to assemble mating parts depends on a "go" condition at the maximum material limits of the parts. The minimum material limits, which are determined by the respective tolerances, are- often not as critical from a functional standpoint. Accordingly, it may be desirable to emplby a combination of Methods A and B in certain conversions by using Method B for the maximum material limits and Method A for the minimum material limits. Alternatively, it may be desirable to round automatically the (converted minimum material limits outside the original limits to provide greater tolerances for manufacturing. 4.5.7 While'the-technique described in 4,5 provides good accuracy of conversion, it will often result in dimensions that are impractical for actual production use. For conversions intended for production, it is usually necessary to round to fewer decimal places and apply design judgment to each dimension to assure interchangeability. 4.6 Other`Units: 4.6.1 Temperature--General guidance for converting tol erances from degrees Fahrenheit to kelvins or degrees Celsius is given below: Conversion of Temperature Tolerance Requirements Tolerance, *F Tolerance, K or C 2 (1) 4 (2) 10 (5) 20 (10) 30 (15) 40 (20) 50 (25) 1 (0,5) 2(1) 6 (3) 11 (5.5) 17 (8.5) 22 (11) 28 (+14) Normally, temperatures expressed in a whole number of degrees Fahrenheit should be converted to the nearest 0.5 kelvin (or degree Celsius). As with other quantities, the number of significant digits to retain will depend upon implied accuracy of the original dimension, for example: 100 5F; implied accuracy estimated to be 2F. 37.7777 2.7777C rounds to 38 3"C. 1000 50F; implied accuracy estimated to be 20F. 537.7777 27.71TTC rounds to 540 30"C.' 4.6.2 Pressure or Stress--As with other quantities, pres sure or stress values may be converted by the principle-given above. Values with an uncertainty of more than 2 % may be converted without rounding by approximate factors: 1 lbf/in2 (1 psi) = 7 kN/m2 = 7 kPa 5. Terminology 5.1 To help ensure consistently reliable conversion and rounding practices, a clear understanding of the related nontechnical terms is a prerequisite. TABLE 9 Rounding Tolerances Inches to Millimetres Original Tolerance, inches at least less than Fineness of Rounding, mm 0.000 04 0.000 4 0.004 0.04 0.4 0.000 4 0.004 0.04 0.4 0.0001 0.001 0.01 0.1 1 1117 DUP050298294 # E 380 5.2 Certain terms used in this standard are defined as foUows: accuracy (as distinguished from precision)--the degree of conformity of a measured or calculated value to some recognized standard or specified value. This concept involves the systematic error of an operation, which is seldom negligible. approximate value--a value that is nearly but not exactly correct or accurate. coherent system of units--a system of units of measure ment in which a small number of base units, defined as dimensionally independent, are used to derive all other units in the system by rules of multiplication and division with no numerical factors other than unity (see Appendix X1.9). deviation--variation from a specified dimension or design requirement, usually defining upper and lower limits (see also tolerance). digit--one of the ten arabic numerals (0 to 9). dimension--a geometric element in a design, such, as length" or angle, or the magnitude of such a quantity. feature--an individual characteristic of a part, such as screw-thread, taper, or slot. figure (numerical)--an arithmetic value expressed by one or more digits. inch-poutid units--units based upon the yard and the pound commonly used in the United States of America afiifci defined by the National Institute of Standards and Tec.i-'i nology. Note that units having the same names in other j countries may differ in magnitude. > nominal value--a value assigned for the purpose of c on- venient designation; existing in name only. precision (as distinguished from accuracy)--the degree of j mutual agreement between individual measurements;.,' namely repeatability and reproducibility. significant digit--any digit that is necessary to define a value or quantity (see-4.3). tolerance--the total amount by which a quantity is; allowed to vary; thus the tolerance is the algebraic difference between the maximum and minimum limits. Bu4 ,.ft3 .Pp p H. ;ib/| quf> 1118 DUP050298295 # E 380 such as d by one and the irica and id Techin other ! of con- iegree of rements, define a rntity is ifference E 380 SELECTED CONVERSION FACTORS To convert from to jjktmosphere (760 mm Hg) ,j'board foot Btu (International Table) fetu (International Table)/b fetu (International Table).-in./s-ft2-F (k, thermal con( ductivity) ij calorie (International Table) Icentipoise scentistokes (circular mil (degree Fahrenheit foot ft2 ft3 ft-lbf ft-Jbf/min ft/s2 gallon (U.S. liquid) horsepower (electric) inch in.2 in.3 inch of mercury (60F) inch of water (60F) kgf/cm2 kip (1000 lbf> kip/in.2 (ksi) ounce (U.S. fluid) ounce-force ounce (avoirdupois) oz (avoirdupois)'/ft2 oz (avoirdupois)/yd2 oz (avoirdupois)/gal (U.S. liquid) pint (U.S. liquid) pound-force (lbf) pound (lb avoirdupois) lbt/in2 (psi) lb/in.3 lb/ft3 quart (U.S. liquid) ton (short, 2000 lb) torr (mm Hg, 0C) W-h yard yd2 yd3 pascal (Pa) cubic metre (m3) joule (J) watt (W) watt per metre kelvin [W/(m-K)] joule (J) pascal second (Pa-s) square metre per second (m2/s) square iiietre (m2) degree Celsius metre (m) square metre (m2) cubic metre (m3) joule (J) watt (W) metre per second squared (m/s2) cubic metre (m3j watt (W) metre (m) square meter (m2) cubic metre (m3) pascal (Pa) pascal (Pa) pascal (Pa) newton (N) pascal (Pa) cubic metre (m3) newton.(N) kilogram (kg) kilogram per square metre (kg/m2) kilogram per square metre (kg/m2) kilogram per cubic metre (kg/m3) cubic metre (m3) newton (N) kilogram (kg) pascal(Pa) kilogram per cubic metre (kg/m3) kilogram per cubic metre (kg/m3) cubic metre (m3) kilogram (kg) pascal'(Pa) joule (J) metre (m) square metre (m2) cubic metre (m3) * Exact multiply by 1.013 25 x 105 2.359 737 x 10~3 1.055 056 x 103 2.930 711 x 10"' 5.192 204 x 102 4.186 800* 1.000 000* x 10~3 1.000 000* 10"6 5.067 075 X 10~10 . rC = (CF -- 32)/1.8 3.048 000* x 10-' 9.290 304* 10~2 2.831 685 x 10"2 1.355 818 2.259 697 x 10~2 3.048 000* x 103.785 412 x !0-3 7.460 000* X 10+2.540 000* X 10" 6.451 600* x i0"` 1.638 706 x 10~5 3.376 85 x 103 2.488 4 x 102 9.806 650* x 104 4.448 222 x 103 6.894 757 x 106 2.957 353 x 10-5 2.780 139 x 10"' 2.834 952 x 10"2 3.051'517 x 10"' 3.390 575 x 10"2 7.489 152 4.731 765 x 10"4 4.448 222 4-.535 924 x 10_1 6.894 757 x 103 2.767 990.X 104 1.60.1 -846 x 10 9.463 529 x 10~4 9.071 847 x 102 1.333 22 x 102 3.600 000* x 103 9.144 000* x 108.361 274 x 10-' 7.645 549 x 10"' 1119 DUP050298296 Condensed Index of Committee D-l Standards--19921 This index references all standards under the jurisdiction of Committee D-i on Paint and Related Coatings and M , plus several others of auxiliary usefulness. It attempts to include what is relevant and exclude what is incidental to the cone nip of each standard. Being designed for Committee D-I usage it omits much of the detailed information provided in the i i more comprehensive index, the latter being intended for users with a broader range of product concern. It's structure employ cross-indexing from specific to general and vice-versa, with the objective of avoiding redundancy while guiding the usci with- dispatch to the desired and related material. The criterion for the selection of index terms is whether they might reasonablv occur to an index user familiar with the technology of organic coatings. Index users encountering errors or other deficieruvs' should report them promptly by writing to ASTM Subcommittee D01.18 in care of ASTM Headquarters. Changes will* be included in the next edition along with entries for new 'standards. Subcommittee chairmen should review the standards under ` their jurisdiction for that purpose. ' 1 This index was developed by ASTM Committee D-i and is not an official ASTM document. It is published for information purposes only. Abrasive blasting profile of blast-cleaned steel, D4417(l) Abrasion resistance air blast abrasive-test D658(l) falling sand/abrasive test. D968(l) Taber Abraser test, D4060(l) wear resistance, of traffic paint, D9I3(I) wet abrasion/scrubbing, 1)2486,4213(1} Accelerated exposure tests See Exposure accelerated Acetaldehyde acetaldehyde, spec., D47W(3) acidity, test, D2086(3) Acetate ester solvents purity, alcohol content, D3545(2) Sa Amyl acetate n-Butyl acetate Ethyl acetate Hexyl acetate Isobutyl acetate Isopropyl acetate Methyl amyl acetate n-Propyl acetate 'Sa Glycol ether acetates Acetic acid (glacial) formic acid in glacial acetic acid. 1)3546(3} specification, D3620(3; Acetone acetone tolerance, of bodied oils, 01950(3) alkalinity, lest, 01614(3) permanganate lime, lest, 01363(3) specification, 0329(3) Acetylene black, See Carbon black Acidity/alkalinity/ (pH) acetaldehyde, spec., D4710(3) acetone, test, D1613,1614(3) chemically cleaned/etched concrete, D4262(l)| electrocoat baths, D4584(l) fatty quaternary ammon. chlorides, D20SK3) formaldehyde solutions, test, D2379(3) hydroxypropyl methylceilulose, D2363(2) tnilliequivalence, electrocoat baths, D4370O) phenol-formaldehyde, D4613(3) pigments, D1208(2) volatile solvents, D1613(3> Add nuinber(vatue) fatty acids, D1980(3) lac resins, test) D29(2) organic coating materials, D 1639(1) pine tars and pine tar oils, test, D856(3) rosin oil, tes^ 1)1131(3) rosin test, 1)465(3).. tall oil, test, 1)803(3),. turpentitie and^pirtene, test, D233(3) i $ a Saponification number Add resistance (of paints/related coatings) clear coatings on aluminum, test, D3260(l) Acrylate esters, purity*, D3362<3) Acrylic acid dimer content, 1^4.41,5(3) specification,^ P446(3) Acrylic emulsion paints. See Artists' Paints Adhesion/Cohesion by cut tape' .test',;D3359(1) Dillon dynometer test, D4796(l) HIPAC coatings, D3730(l) portable tester, pull-off strength, D454I(1) prepainted fabricated metal, D4145(l) scrape test on smooth surfaces, D2197(l) traffic marking paints, materials,.D4796(l) zinc-rich primer on steel, D4146(l) Air blast abrasion tester, D658(l) Alcohol resistance, furniture lacquer, D257I(1) Alcohol solvents See Amyl alcohol, D319(3) n-Dutyl alcohol (I-Butanol), D304(3) sec-Butyl alcohol (2-Butanol), D1007(3) 2-EthyIhexanol, D5G08(3) Isobutyl alcohol (isobutanol), D1719<3) Isopropyl alcohol (isopropanol), D770(3) Methyl isobutyl carbinol, D2635(3) Methanol (Methyl alcohol), D1152(3) n-Propyl alcohol (n-propanol), D3622(3) Aldehydes, purity, test, D2192(3) Algae (algal growth) See Biodeterioration Aliphatic hydrocarbon solvents See Mineral (petroleum) spirits VM&P naphtha Alkali resistance, of varnishes, DI647(1) Alkyds/alkyd resins carboxylic acids content, D2455(2) fatty acids content, D1398(2) isophthalic acid content, D2690(2) phthalic anhydride content, D563-, D1306(2) polyhydric alcohol, D1615, 2456, 2998(2) Alkyds/alkyd resins (cont'd) rosin add content D1469(2) ' silicon content D3733C2) test methods, selection of, D2689(2) unsaponifiable matter content 01397(2) Sa PainfsJ solvent-reducible Aluminum (metal surfaces) aad/mortar resistance,of coatings,D3260(l) preparation for painting,;D1730, D173K1) Aluminum powder and paste sampling/testlng, D480(2> specification, T>962(2) Aluminum silicate (anhydrous) analysis, D718(2) - specification, D 3619(2) Sa Pigments,general properties Aluminum silicate (hydrous) analysis, D718(2) specification, D603<2> Sa Pigments, general properties Amidoamines, See Fatty amines Amino resins free formaldehyde content, D1979(3) test procedures, practice, D4277{2) nitrogen content D'1013(2) solvent tolerance test, D1198(2) Amines/amine values Set? Fatty amines Fatty quaternary/amine chlorides Amyl acetate, synthetic primary, D3540(3) Amyl alcohol (synthetic), spec., D319(3) Analysis See Chemical analysis Aniline sampling and handling, practice, D3436 (3) specification, D3264(3) 1120 h* I DUP050298297 Condensed Index of Committee D-1 Standards Aniline point dipentene, related terpene solvents, 0801(3) petroleum hydrocarbon solvents,D6U(3) Anti-corrosion pigments See Basic lead silicochromate Red lead Strontium chromate Tribasic lead phosphosilicate Zinc chromate Zinc dust Zinc hydroxy phosphite Anti-fouling pigments See Copper powder Cuprous oxide Mercuric oxide Anti-fouling paints, submergence test, D3263(l) erosion test, high velocity water, D4938(l) erosion test, rotating drum, D4939(l) organotin release rate, 05108(1) Anti-fungal pigments See Calcium borosilicate Zinc Oxide Antimony oxide analysis, 02350(2) analysis by spectrophotometry, D3717(l) $a Pigments, general properties Anti-sag meter, multinotch blade, D4400C1) Applicators, film See: Film application/applicators Architectural paints and coatings block resistance, 04946(1) color permanence, white enamels, 01543(1) brushability (brush drag), 04958(1) efflorescence of wall paints, 01736(1) him,failures, exterior latex paint, D1848(l) film porosity, 03258(1) freeze-thaw resistance, 02243(1) gloss or sheen uniformity, 03928(1) gloss terminology & definitions,in prep, guides for testing architectural coatings: exterior paints, solvent-bomc, 03323(1) water-borne, D3129(l) flat paints, sotvent-bome, 03323(1) water-borne, D2431(l) floor paints, solvent-borne, 03383(1) water-borne, 03358(1) gloss and S/G, solvent-bome, 03425(1) water-borne, D4540(l) high performance (HIPAC), 03730(1) solvent-bome (general), D5146(l) water-borne (general), in prep, guide for purchasing: state and institutional, 03927(1) hiding power: brush application, visual, 0344(1) drawdown, reftectometric, 02805(1) roller application, visual, in prep, wet-to-dry hiding change, DSO07(1) leveling, D4062O) minimum film formation temp., 02345(1) package stability, 01849(1) porosity of films, 03258(1) print resistance, D4207(l) roller spatter, resistance to, 04707(1) sag resistance, 04400(1) washability: soilant, mechanical test, D3450(l) practical multi-stain test, 04828(1) wet abrasion (scrub) resistance: scrub-to-failure test, 02486(1) weight-loss test, 04213(1) Aromatic hydrocarbon solvents See High-flash aromatic naphtha Toluene Xylene Arsenic content, in paint, D2348(l) Artists' paints drawdowns, preparation of, D4941(l) labeling for health hazards, D4236(l) lightfastness of pigments, D4303(l) specifications acrylic emulsion, D5098(l) oil, acrylic, alkyd, resin-oil, 04302(1) water colors, 05067(1) tinting strength, 04838(1) Asbestine See Magnesium silicate Atlas Weatherometer, 05031(1) Automotive painting spray transfer efficiency, D5066(1) Bacterial resistance See Biodeterioration Baking, effect of overbaking, 02454(1) BalL drop method, for viscosity ,01343(2) Barium sulfate (barite, barytes) analysis, 0715(2) specification, D602(2) 5 a Pigments, general properties Basic carbonate white lead analysis, 01301(2) specification, 081(2) 5 a Pigments, general properties Basic lead silicochromate analysis, 01844(2) specification, D1648(2) S a Pigments, general properties Basic sulfate white lead analysis, D1301(2) 5 a Pigments, genera! properties Bend testing mandrel bend test, 0522(1) Berlin white See Basic carbonate white lead Biocidal pigments See Anti-fouling pigments Anti-fungal pigments Biodeterioration (microbiological attack) emulsion paints in container, 02574(1) paint films: discoloration - exterior exposure, 03456(1} mold - environmental chamber, 03273(1) removal of fungal/algal growth, D4610 (1) soil/dirt/fungal accumulation, 03274(1) 5 a Anti-fouling paints Bituminous materials water content, by distillation, D95(l) Black box exposure test accelerated outdoor exposure, D4141C1) Black iron oxide See Iron oxide black Black pigments See Bone black Carbon black Iron oxide black Lampblack Blade applicators See Film application/applicators Blanc fixe Sec Barium sulfate Blast-cleaned steel (abrasive) profile of steel surfaces, D4417(l) Bleeding (bleed resistance) See Pigments-general properties Traffic paint Blistering (Blister resistance) pictorial standards/evaluation, D714(l) water condensation test, D4585(l) water fog test D1735<1) Blocking (block resistance) of architectural coatings, D4946(l) lacquers on metal substrates D3003(l) on wood substrates D2793(l) Blue pigments, mixture, analysis of, D1135(2) 5a Iron blue Phthalocyanine blue Ultramarine blue Boiled oils (drying) See Linseed oil Bonding strength. See Adhesion/cohesion Bone blade solvent extractable matter, D305(2) spec., D210(2) Sa Pigments, general properties Break test. See Fatty oils Bronze powdery- See Gold bronze powder Brookfield viscometer. See Viscometers Brown pigments See Iron oxide Sienna, raw and burnt Umber, raw and burnt 5 a Pigments, general properties Brunswick blue See Iron blue Brunswick green See Chrome green Brushability (Brush drag) Manual application test, 04958(1) High shear (ICI) viscosity, D4287<1) Brushes, paint See Paintbrushes , Bubble time method See Viscometers Burning Characteristics of liquid ingredients Equilibrium method, closed cup flash/no flash, D,3934(3) flash point, 03943(3) Pensky-Martens (dosed cup), D93(l,3) Seta flash tester (closed cup), D3278(3) Seta flash tester (open cup) 04206(3) Sustained burning test, D4206,4207(3) Tag,dosed cup, flash point, 056(3) Tag,-open cup, flash/fire point, D1310(3) Wick test, D4207(3) of paints/coatings char index, cabinet method, 01360(1) 2-foot tunnel method, 03806(1) Burnt sienna/umber See Sienna, burnt and raw Umber, burnt and raw 1- Butanol See n-Butyl alcohol 2- Butanol See sec-Methyl ethyl alcohol 2-Butanone See Methyl ethyl ketone 2-Butoxy ethanol, spec., D330(3) Butyl acetate alcohol content/purity, D3545(3) specification, D4615(3) Butyl, acrylate purity test, D3362<3) ~~~ specification, 03547(3) Butyl acrylate/methacrylate monomer content of latexes, 04747(2) n-Butyl alcohol, specification, D304(3) sec-Butyl alcohol, spec., D1007(3) Butyl glycol See 2-Butoxyethanol Butyral content cellulose acetate butyrates, test, D817(2) Cadmium content in low concentrations in paint, 03335(1) Calcium borosilicate analysis, 04487(2) specification, D4288(2) Sa Pigments,general properties Calcium carbonate specification, D1199(2) $a Pigments, general properties Calcium content cellulose pulp (from wood/cotton), 04085(2) paint driers, by EDTA method, D2613(3) Calcium paint driers Sec Driers 1121 W> DU P05 02 982 98 Condensed Index of Committee D-1 Standards Carbon-arc lamps See Exposure, accelerated Carbon black pigment for paint, spec., 0561(2) solvent extractable material, 0305(2} Sa Pigments, general properties Carboxyl contend of cellulose, D1926{2) Carboxymethyl cellulose, sodium, 01439(2) Carboxylic acids, identification in alkyd resins, D2455(2) Castor oil, dehydrated specification, 0961(3) diene value, 01358(3) Sa Fatty oils Castor oil, raw specification, 0960(3) hydroxyl content, 01957(3) Sa Fatty oils Cauiking/glazing compounds and sealants viscosity, falling-rod-viscometer, 04040(1) Cellulose and cellulose derivatives acetate/ butyrate and proprionate, D817(2) akohol-benzene-soluble content, D1729(2) ashing, test methods, D3516(2) carboxyl content, test, 01926(2) cellulose acetate, test, 0871(2), 0365(2) cellulose nitrate, See Nitrocellulose chain length uniformity,-01716(2) chlorine content^test, D264l(2) chromatographic analysis, 01915(2) cold check resistance, lacquers, 01211(1) definition of terms, 01695(2) dichloromethane-soluble matter, D3971(2) ethoxyl substitution in cellulose, 04794(2) ethyl cellulose (EC) plastics, 0914(2) .ethyl cellulose pulp, metals content, D40S5(2) hydroxyethyl cellulose, 02364(2) hydroxypropyl cnerhylcellulose, D'2363(2) hydroxypropyl substitution, 03876(2) methoxy substitution, 03876(2) methylcellulose, test methods, 01347(2) moisture content, test, 01348(2) nitrocellulose. See Nitrocellulose silica content, test D2438(2) sodium carboxymethylcellulose, 01439(2) solubility in sodium hydroxide, 01696(2) sulfur content, D2929C2) viscosity, ball-drop method, 01343(2) viscosity, intrinsic, 01795(2) volatile/non-volatile of solutions, 04209(2) Centrifuge, See Vehicle separation Cerium paint driers; See Driers Certification of conformance, form, 05063(4) Chalk, See Calcium carbonate Chalking, exterior paints, D6S9, 04214(1) Channel black See Carbon black Char index See Burning characteristics Checking (check resistance) exterior paints, test 0660(1) S a Cold checking Chemical Analysis See Pigments, analysis White pigments, analysis Chemical resistance, to: acid & mortar, of coated aluminum, 03260(1) alkali, of varnish films, 01647(1) alcohol, of wood furniture lacquers, D257KI) household chemicals, of coatings, 01308(1) China clay See Aluminum silicate (hydrous) Chinese blue See Iron blue China red See Chrome orange Chinese white See Zinc oxide Chip (chipping) resistance of coatings, 03170(1) of traffic paint, 0913(1) Chlorinated phenol preservative content in wood products, D2921(l) Chlorine content cellulose, test, 02641(2) epoxy resins/compounds, test, 04301(2) hydrolyzablc,of liquid epoxy resins, 01726(2) polyvinyl chloride, 01156(2) toluene diisocyanate, D1638(3) total, of liquid epoxy resins, Dl847(2) Chromaticity, See Color Chromatography See individual analysis references Chrome green analysis, 0126(2) specification, 0212(2) Sa Pigments (general properties) Chrome yellow and orange analysis, D126(2) specification, 0211(2) Sa Pigments, general properties Chromium content- low concentrations in air particulate filter samples, D4358(2) in paint, 03718(1) Chromium oxide green analysis, 0126(2) specification, D263(2) Sa Pigments (general properties) Chromium pigments See Chrome green Chrome yellow and orange Chromium oxide green. Lead silicochromate. Strontium chromate Zinc chromate CIE color system Sec ` Color-opaque materials Citron yellow See 1 Strontium Chromate Clarity/cleanliness of paint and ink liquids, D2090 (3) Clay, See Aluminum silicate Cloud point aromatic hydrocarbon solvents, 04790(3) Coalescence latex paint films, low temperature, 03793(1) Coarse particle analysis See Dispersion (of pigments) Particle size (analysisMistribution) Cobalt content paint driers, by EDTA method, 02373(3) paint, in low concentrations, D3335(l) liquid drier, analysis, DS64(3) Coconut oil. See Fatty acids, tests, specs. Coefficient of friction See Slip resistance Coefficient of retroreflection See Retroreflection/retroreflectors Coffee stains, resistance to of furniture lacquer, 02571 (1) Cohesion, See Adhesibn/Cohesion Coil coatings wire-wound bar application, 04717(1) guide for testing, D3794(l) Cologne yellow. See Chrome yellow Cold checking of nitrocellulose lacquers, D121K1) Color See Color* opaque materials Color retention Color- transparent liquids and solids Color--opaque mati CIE color system, color differenci u Colour Index, arr i ^ defining and evaluate* evaluating color efiah metamerism, wuirf-<L Munsefi system, 01534 tristunulus valu 0, Dj visual evaluation, of^ Color retention discoloration: microbiologica dear coating j' 'umtgft household chemie^^S white architectural uw** light fastness tf i pigments in arh ri jftanfL-, printed malt.r, ' Color- fcranspatent, hquidiriutT Gardner color scik standard solutions fepOTl caramd/ph t et5Mv platinum-co nil 9 .<!( Dlid Compatability, coating, Concrete and masonn testpanJ^rf pH, chemically Jc.u stirface cleaning (for Conditioning^nv irnnmunf/tor Conductance and cc nduUiVitv $ of electrocoat b rihs 013^91 >) Cone-and-plate-v <Svometersr'^ See Viscometere-j<lCjt 3 : Conformance/certititaiion 0u Corqugated-oils ; i ^ *ir See Dehydrated itVtar^ui ' Oitick.i oil ` Tung oil Sa Fattyo.l Consistency, by Stomu r v Contrast ratio hiding power by ; Copal content, of l See Shellac - i.otMi i '*i Copper content -r cellulose pulp (fromiwociutf-otn copper pigments, test. 194^21 pine tars and pine tar Nik Copper corrosion in aromatic soivents,!0i *9(3) in dipentene & related in petroleum products. D.1MK3>V Sa Exposure test. Copper phthalocyanine bfite'e ^ See Phthalocyamne hluef Phthalocyanine green Copper powder analysis, 0283(2) specification; 0964(2) ,, Sa Pigments, general Com oil. See Fatty acids - k-.t''. Corrosion resistance See Expo^ur*?/^ Cotton seed oil < See Fatty acids - tests, socuUid^^aBj%f Covers, paint roller See - Vo nl roJ*S^CCj^jjjlS Cracking (crack resistance) exterior paints, evaluating* I >661(1)^ mandrel bend test, 0522(1) ` si Cross-cut, cross-hatch taj * t adhesion of paint, test/ 0355*1(1^^ Cuprous oxide analysis, D283(2) specification, 0912(2) 1 \ * Set* Pigments, general yting,* ar4i jitine anf lEion effiS pvderqo[ gent reste JdfoSeej . tone alcq. tjnes. See | ||itaceoUs| phth^ ` jtmelftajf mas chrc4 fene glyt j||DynftE| goti rm [dose ni| . jilose.ruj - 1122 DU P050298299 Condensed Index of Committee D-1 Standards time, thermosetting resins,. D4640(2) Sa Drying/curing tain coating, water reducible, D4712G) k chrome yellow See Chrome yellow and orange itions of terms elated to paint, varnish, etc., 016(1,2,3) ydrated castor oil See Castor oil, dehydrated Fatty acids - tests, specifications ity--apparent (bulk) ydroxyethelcellulose, 02364(2) ydroxypropyl methylcelluiose, 02363(2) ethylcellulose, 01347(2) odium carboxymethvlcellulose, 01439(2) ttsity- true 'pentene/terpene solvents, D801(3) industrial aromatics, 02935(3) aints and related coatings, D1475C1) X liquids, 01963(3) igments, tests, D153(2) ie oil, 0802(3) e tars and oils, 0856(3) rpentine and pinene, D233(3) position efficiency of powder coatings, 03451(1) tergent resistance, 02248(1) ew cycle. See Exposure tests - accelerated cetone alcohol, spec., D2627(3) famines. See Fatty diamines iatomaceous silica. See Silica ibutyl phthalate, spec., D608(3) ichlormethane, determination of by gas chromatography, D4457(l) iethlene glycol, spec. D2694(3) illon Dynamometer, See Adhesion/cohesion Hution ratio/Dilutability cellulose nitrate solutions,D1720(3) cellulose nitrate, with toluene, D301(2) resin solutions, 05062(3) [methyl ketone, See Acetone ip application water reducible coatings, 04717(1) 'pentene (and related terpene solvents) sampling and testing, 0801(3) : {propylene glycol specification, 02696(3) ipropylene glycol monomethyi ether (DPGME) specification. 04836(3) purity, 04773(3) ip-type viscosity cups. See Viscometers irectional reflectance See Reflectance and reflectivity irt/Soil resistance exterior white coatings, 03719(1) practical washability,-04828(1) f washability, mechanical test, D3450 Disbonding--cathodic pipeline coatings, cyclic temperatures, G42(l) pipeline coatings, test, G8(l) Discoloration See Color retention Dispersion/fineness of grind (of pigments) coarse particles by sieve test, D185(1), (2) dispersion stability, phthalo blue,.D963(2) in pigment-vehicle systems, 01210(1) in printing inks, NPIRI grindometcc, 01316(1) in titanium dioxide slurries, D3926(2) Distillation dipentene, terpene solvents, D801(3) distillation range, 01078(3) ethyl acetate, spec.,D4614(3) in vacuum, solvent-type paints, D3272G) petroleum products, 086(3) pine oil, 0302(3) pine tars and tar oils, D856<3) turpentine and pinene, D233(3) Dolomite, See Calcium carbonate Draft test, varnish films, D1643(1) Drawdown bars and rods See Film application/applicators Draw-down tests, multi-notch applicators leveling characteristics of paints, 04062(1) leveling of paints, D2801 (discontinued) sag resistance of paints, 04400(1) Driers calcium/zinc content, EDTA, 02613(3) cerium content, test, 03970(3) clarity/cleanness, visual, D2190(l,3) cobalt content, EDTA method, D2373(3) iron content, EDTA method, D2374(3) manganese content, EDTA method, D2375(3)'* rare earths content, EDTA method, D3989(3) selection of test methods, D564(3) specification, D600(3) vanadium content, EDTA method, 03988(3) volatile/nonvolatile content, D4140(3) zirconium content, EDTA method, D3%9(3) Drop black. See Bone black Dry film thickness,$er Film thickness, dry film Drying oils. See Fatty oils Drying ./curing cellulose nitrate, D30K2) MEK resistance, zinc-rich primers, D4752G) room temperature, film formulation, D1640G) shellac varnish, 01650(2) temperature during curing by I.R., D3259(l) thermosetting resins, cure time, 04640(2) ultra-violet cured coatings, D3732(l) Durability, See Exposure tests Dutch white, Se* Basic carbonate white lead Dynamic immersion tests of Anti-fouling paints, D4938, 4939(1) Dynamometer testing See Adhesion/cohesion Earth pigments See Ocher, Sienna, Umber Eccentric wheel, See Film thickness gages EDTA method, paint driers calcium content, D2613{3) cobalt content, 02373(3) iron content, D38Q4{3) lead content, D2374(3) manganese content, D2375(3) rare earths content, D3989(3) vanadium content, 03988(3) zinc content, 02613(3) zirconium content, D3969(3) Efficiency See Deposition efficiency (powder coatings) Transfer efficiency-spray application Efflorescence exterior latex paints, D1648{1) interior wall paints ,01736(1) Elasticity, of varnishes, test, D 1642(1) Electrical insulating solids shellac specifications, D784(2) shellac, test methods, 0411(2) Electrocoat baths Add /base milliequivalency, D4370<1) Guide for testing, D1978(1) pH measurement, D45S4(1) Electrostatic deposition See Powder Coatings Electrostatic spray water-reducible coatings, D4712(l) Elongation mandrel bend test, D522(1) tensile strength/stiffness,free films, D2370(l) Emulsion vehicles (for paints/related coatings) freeze-thaw resistance, 02243(1) minimum film formation temp., 02354(2) So Latex vehicles Environment standard conditioning for testing coatings, 03924(1) thermosetting (molding) compounds, 01013(2) Erosion resistance of exterior paints, 0662(1) Se Abrasion resistance Anti-fouling paints Ester solvents See Acetate ester solvents Epoxy (EP) resins bond strength, traffic mark'g mat's, D4796(l> chlorine content, D1847,4301(2) epoxide equivalent wt., 01652(2) epoxy content, Dl652(2) guide for testing, 04142(2) hydrolyzable chlorine content, 01726(2) Ester value of solvents and thinners, 01617(3) Ether-alcohols See Glycol ethers 2-Ethoxy ethanol, specification, D331(3) 2-Ethoxyethyl acetate alcohol content/purity, 03545(3) specification, D3728(3) Ethyl acetate alcohol content/purity, 03545(3) specification, 04614(3) ^ Ethyl acrylate ethyl acrylate, spec., D3548<3) purity, D3362(3) Ethylene glycol specification, 02693(3) Ethylene glycol monobutyl ether See 2-Butoxyethano! Ethylene glycol monoethyl ether , ___ ,, See 2-Ethoxy ethanol Ethylene glycol monomethyl ether Sec 2-Methoxy ethanol 2-EthylhexanoI, analysis, 05008(3) 2-Ethylhexy! acrylate, spec., D354K3) Ethyl silicate, zinc-rich primer v MEK resistance, 04752(1) Evaporation rate, volatile liquids, 03539(1) Exposure - accelerated-corrosive environment cyclic salt spray/humidity/cold 02933(1) filiform corrosion on steel, D2803<1) method for evaluating corrosion, 01654(1) Exposure - accelerated -water/humidity/light black box/Fresnel reflector rack, D4141Q) carbon arc lamp - dew cycle, 03361(1) carbon arc lamp/unfiltered, 0622(1) carbon arc lamp, enclosed, Atlas, 05031(1) controlled condensation, 04585(1) fluorescent UV/condensation, D4587C1) 100% humidity chamber, D2247 (1) wood panel substrates, 0356 (06. xenon arc/water spray, G26(l) 1123 X DUP050298300 Condensed Index of Committee D-1 Standards Exposure testing* exterior house paints on new wood, Dl006(l) paints on steel surfaces, D1014,5065(1) quantifying dirt collection, 03719(1) recording results on standard forms, D1150(1> wood panel substrates, D358(l) Extender pigments See Aluminum silicate (day) Barium Sulfate (barytes) Calcium carbonate (whiting) Magnesium silicate (talc) Mica Pumice Silica, diatomaceous Exterior paints and coatings See Architectural paints and coatings. Exposure testing Factory applied finishes S ee Industrial finishes, water-borne Wood finishes v See Color retention Falling-rod viscometer See Viscometers Falling sand method. See Abrasion resistance Fatty adds--general definition of terms, 01467(3) sampling, 01466(3) testing methods, 02575(3) Fatty acids--specifications coconut oil, 01841(3) com oil, 01842(3) cottonseed oil, 01843(3) dehydrated castor oil, 01539(3) linseed oil, 01538(3) soybean oil, 01537(3) tall oil, D19$4<3) Fatty acids--tests add value, 01980(3) ash content, 01951(3) clarity/cleanness, D2090(l, color after heating, 01981(3) fish oil content, D3725(3) Gardner color scale, 01544(1,2,3) hydroxyl content, 01957(3) iodine value, 01959(3) rosin acid content, 011240(3) saponification value, D1962(3) solidification point, 01982(3) spsdfic gravity, test, D1963(3) titer test, 01982(3) unsaponifiable matter, 01965(3) Fatty acids content alkyd resins, D1398(2) methyl esters, 01983, 3457(3) solvent paints, 02245(3) tall oil rosin, test, D1585C3) tall oil test, 0803(3) Fatty amines, amidomines, diamines amine content, D2083(3) amine values, 02073,2074(3) iodine value, Wijs, 02075(3) isocyanates test, 01638(3) non-amine content, 02082(3) test methods, amidomines, D207K3) water content, D2072(3) Fatty nitrogen compounds identification in solvent paints, D2245(3) non-amine content, D2082(3) test methods, D2071(3) water content, test, D2072(3) Fatty oils (drying oils) absorption (by pigments), 0281,1483(2) Fische, reagent method (forwafer v Fish fir f311 Fis*er re*St treijjJr? acetone tolerance (heat-bodied oils), D1950(3) ash content, 01951(3) break test, 01952(3) darity/cleanliness, visual, 02090(1, 3) color after heating, test, D1967(3) conjugated diene value, 01358(3) content, of solvent paints, 02245(3) definition of terms, D555(3) film formation rates, drying, 01640(1) Gardner color scale, 01544(1,2,3) Frsh ml m drying oils andfe ,,,,d. So Fatty oils # Flake brass See Gold bronze po^dor ,,r * '** Flaked powders \ m t- S"u-^U7il1U^ POYvdera''rf FastrtC i. 1.V _ F akewhrie See Basic carbonat. whhSr^tV Flaking (flake resistance) , exterior paints D722(1) Flammability/fire retardancy See Burning characteristics l'VJl gel time, test, 01955(3) iodine value, test, 01959(3) loss on heating, 01960(3) Flash point--liquids See Burning characteristics Flat paints, interior JkujA * sampling, D1466(3) saponification value, 01962(3) solvent-borne, test guide, 03323 water-borne, test guide, 02931 * 1^281 selecting test procedures, guide, 04140(3) Flexibility specific gravity at 25/25'C, test, 01963(3) Fatty oils (drying oils) - (cont'd) impact resistance, D2794(l) mandrel bend test, D522(l) * ^fiSSIS? testing methods, D555(3) unsaponifiable matter content, 01965(3) unsaturation, Rosenmund-Kuhnhenn, 01541(3) on prepainted metal sheets,D4145(t) * r ^ Flocculation - of pigments, test for, DOr^l : M Floor paints/coatings * unsatuxation, Wijs method, D1959(3) clear floor sealers, 03546(1) i$* S a Castor oil, raw * solvent-borne, test guide, D33R (<> * . Castor oil, dehydrated water-borne, test guide, 03358(1) - Fish oil Flow and flow rate < Linseed oil See Rheological properties *l Oiticica oil Foots, in raw linseed oil Safflower oil gravimetric method, 01966(3) Soybean oil Sunflower oil Tall oil volumetric method, 01954(3) Ford cup, See Viscometers Formability Tung oil Impact-Wedge bend test, D3281C') Fatty quaternary ammonium chlorides zinc-rich primer on steeL 04146(1) acid value, tests, 02076(3) Formaldehyde amine value, test, 02076(3) acidity test, D2379(3) ash content, test, 02077(3) iodine value, 02078(3) in amino resins, D1979(3) iron content, test, D2QS7(3) nonvolatile matter, D2079(3) methanol content, test, 02380(3) molecular weight, D208O(3) specification, 02378(3) pH, test, D2081O) Forms water content, 02072(3) certification of conformance, 05063(1) recording exposure test results, 0115011) Ferric oxide/Ferrite See Iron oxide pigments Ferrous iron in iron oxides, D3872(2) Field identification/analysis Fouling See Anfi-fouling paints Free films (organic coatings) of structural coatings, 05043(1) preparation, tensile properties, D2370(l) Filiform corrosion resistance preparation of, 04708(1) of organic coatings, 02803(1) Freeze - thaw resistance 5 a Exposure tests-accelerated-corrosive multicolored lacquers, D2337(l) Film application/applicators artists' paste paints, practice, D4941(l) blade applicators, D823(l) producing uniform films, D823(l) water-borne paints, 02243(1) SeeFrenchblue Iron blue SeeFrench chalk Magnesium silicate SeeFrench ocher Ocher wire-wound (Meier) rods, D4147(1) Fresnel reflector rack exposure Film formation, emulsion vehicles accelerated outdoor metal exposure 04141(1) minimum temperature (MFFT), 02354(2) Friction, static coefficient. See Slip resistance Film porosity. See Porosity Fuel oil / solvent resistance Film thickness gages of traffic paints, 02792(1) dry films by incision cut, Tooke gage, 04138(1) Fungicidal (fungistatic) pigments See Anti-fungal pigments on non-ferrous metals (eddy), 01400(1) on steel, magnetic gage, D1186 using micrometers, 01005(1) Fungus resistance/fungirides See Biodeterioration SeeFurnace black. Carbon black wet films eccentric wheel, D1212(l) Interchemical and Pfund gages, D1212(l) notched gages, 04414(1) Galvanized surfaces Films, organic coatings. See Free films See Steel panels/pipe/tube/sheet Fineness of grind (dispersion) Gardner-Coleman method See Dispersion oil absorption of pigments, 01483(2) Fire retardancy/flammability Gardner color scale S ee Burning characteristics transparent liquids, test, 01544(1,2,3) % 1124 DUP050298301 Condensed Index of Committee D-1 Standards er-Holdt viscometer tubes ee Viscometers ecking, draft test, varnish films, D1643(l)| ine resistance, of traffic paints, D2792(l) ;~e 'ng oils, test, D1955(3) ^oLds, test D2870(3) 'panels 'ace prep for testing coatings, D3891(l) s beads (in traffic paint) f4ysis for D4797(l) 5 e analysis, D1214(2) | for roundness of, 01155(2) ; (specular) and Sheen nge, washability of coatings, 04828(1) iect of household chemicals, 01308(2) -s differences, visual evaluation, 04449(1) i of high gloss finishes, 04039(1) i gloss, goniophotometer, test, E430<1) easurement of gloss and sheen, 0523(1) erances, conformance evaluation, 03134(1) ifonnity of brushouts, test, 03928(1) paints \-See Architectural paints jqerin--high gravity pnpling/testing,.01258(3) " fication, m257(3) cidal ethers 'orine content in epoxy resins, 04301(2) els See Diethylene glycol, 02694(3) Dipropylene glycol, D2696(3) Ethylene glycol, 02693(3) Hexylene glycol, 02636(3) Propylene glycol, D2695(3) col ethers Dipropylene glycol monomethyl ether Ethylene glycol butyL ether Ethylene glycol ethyl ether Propylene glycol monomethyl ether col ether acetates See Ethylene glycol ethyl ether acetate Propylene glycol methyl ether acetalej old bronze powder analysis, 0283(2) Specification, D267(2) S a Pigments, general properties i pigments Chrome green Chromium oxide green Phthalocyanine green nd, of pigment, dispersions See Dispersion/fineness of grind "dometer, NPIRI See Frinlinginks Dispersion/fineness of grind ide for assessing aged coatings cn steel, 05065(1) painting inspectors, metal substrates,D3276(l) uides for testing (selection of methods) See Architectural paints and coatings Coil coatings Electrocoat baths Epoxy resins Industrial finishes Lacquers Latex vehicles Powder coatings Solvents um rosin See Rosin [aiogenated solvents analysis for, in paint, D4457(l) Halo-silane coated glass plates for preparation of free films, 04708(1) Halphen-Hicks test rosin content of varnishes, 01542(1,2) Handling material See Materials handling Hardness testing of organic films Knoop indentation tester, KHN, D1474(l) Koenig pendulum test, D4366(l) pend! test, D3363<1) Persoz pendulum test, D43660) Pfund indentation tester, PHN, D1474U) Sward rocker test, 02134(1) Hazards, fixe and health handling analine, 03436(3) handling cresylic acid, phenol, 03852(3) handling naphthalene, D343B(3) in protective coatings, D3630(l) labeling art materials, 04236(1) Haze See Gloss Heat resistance of organic coatings on steel, D2485 (1) effect of overbaking, 02454(1) Heatset-type printing inks non-volatile content, 04713(1) Hegman scale fineness of dispersion, pigments, D1210C1) Hematite See Iron oxide red n-Heptane flash/fire point of liquids, test, 01310(3) Heptane miscibility See Miscibiity Hexanes commercial, specification, 01636(3) Hexyl acetate, spec,, 05137(1) Hexylene glycol, specification, 02636(3) Hiding power (of paints/coatings) brushouts, visual, relative, 0344(1) drawdowns, reflectometry, 02805(1) roller application, practical, visual. In Prep, wet-to-dry change, visual, 05007(1) High-flash aromatic naphthas, 03734(3) High performance (HIPAC) coatings, 03730(1) High-purity (reagent) water, spec., D1193(3) High shear (IC1) viscosity, 04287(1) S a Brushability Horizontal pull test, static friction, 04518(1) Household chemicals, resistance to, of organic coatings, D1308(l) House Paints See Architectural paints Humidity resistance, of coatings humid-dry cycling, on wood, D3459C1) humidity, on steel, D2247(l) humidity-thermal cycle on steel, D2246(l) Sa Water resistance Hunter, visual gloss differences, 04449(1) Hydrocarbon solvents See Aliphatic hydrocarbon solvents Aromatic hydrocarbon solvents Solvents, general test procedures Hydroquinone content in vinyl acetate, D2193(3) Hydroxyethylcellulose, testing, 02364(2) Hydroxyl content cellulose acetate, D871(2) cellulose acetate, butyrate, D817(l) fatty oils and acids, 01957(3) Hydroxy prcpyi methylcellulose, 02363(2) Hydroxypropyl substitution in cellulose ether products, 03876(2) ICI cone/plate viscometer, D4287(l) Sa Brushability Impact resistance , flexibility test, 02794(1) Imprinting See Print resistance Inclined plane test, static friction, D4513U) Indentation hardness See Hardness Testing Index of refraction See Refractive index Indexes, specialized, of standards and tests Architectural coatings, 02833(1) Sa Guides for testing Indian red See Iron oxide red Industrial finishes water-borne, test guide, D1712(l) Inert pigments See Extender pigments Infrared pyrometry (thermometers) for wood coatings, cure cyde, 03259(1) Infrared spectrophotometry, analysis See Spectrophotometry--infrared Ink,Inkometer, See Printing Inks Inspection of paint application work guide for inspectors, D3276(l) Interchemical Film Thickness Gage See Film thickness gages Interior paints See Architectural paints Interlab testing See Statistical methods Iodine value, tests Drying oils,Rosenmund-Kuhnhenn, 01541(3) fatty amines, Wijs test, D2075(3) fatty quaternary ammon. chlorides, 02078(3) lac resins, test, D29(2) Wijs test, 01959(3) Iron blue ** analysis; D1135(2) specification, 0261(2) Iron oxide blade natural/synthetic-analysis, D3672(2) synthetic., spec., D769(2) See Pigments, general properties Iron oxide brown (natural) analysis, 050(2) specification, 03722(2) Sa Pigments, general properties Iron oxide brown (synthetic) analysis, D3872(2) specification, D3724C2) Sa Pigments, general properties Iron oxide red (natural) analysis, 050(2) spedfication, 03722(2) Sa Pigments, general properties Iron oxide red (synthetic) analysis, 050(2) specification, 03721(2) Sa Pigments, general properties Iron oxide yellow analysis, 050(2) specification, D768(2) Sa Pigments, general properties Iron paint driers See Driers Iron Oxides, ferrous iron content, 03872(2) ISO flow cups. See Viscometers Isobutyl acetate ' alcohol content/purity, D3545(3)( Isobutyl acetate (95% grade), spec., D1718(3) Isobutyl alcohol, specification, D1719(3) Isocyanates foam raw materials, test methods, 01638(3) isocyanate groups in urethanes, D2572(2) Isophorone, specification, 02916(3) Isophthalic acid content alkyd and polyester resins, test, D2690(2) Isopropanol See Isopropyl alcohol Isopropyl acetate alcohol content/purity, D3545(3) Isopropyl acetate (99% grade), spec., D3131(3) Isopropyl alcohol, spedfication, 0770(3) Kaolinite, Kaolin Sec Aluminum silicate Karl Fischer reagent, water content, 04017(1) Kauri-butanol value, D1133(3) 1125 mmmm If-fv DUP050298302 Condensed Index of Committee D-1 Standards Ketones Lieberman-Storch test methyl n-amyl ketone, spec., D436G(3) rosin content of varnishes, 01542(1,2) purity, test, D2192(3) Lightfastness Ketone solvents of printed matter, 03424(1) See Acetone, D329(3) of pigments used in Artists' Paints, D4303(l> Diacetone alcohol, D2627(3) Sa Artists' paints Isophorone, D2619(3) Color retention MethyLamyl ketone, D4360(3) Umonite See Ocher Methyl ethyl ketone, D740(3) Linseed oil Methyl isoamyl ketone, D2917(3) boiled, specification. D260(3) Methyl isobutyl ketone, D1153C3) raw, specification, 0234(3) Knife test, for paint adhesion, D3359(1) Sa Fatty oils Knoop hardness tester, 01474(1) Foote In raw linseed oil Koenig pendulum test, hardness, D4366(l) Oil absorbtion (ofpigments) 5 a Hardness testing Fatty adds - teste, specifications Labeling Liquids, art materials for health hazards, 04236(1) clarity/cleanliness, visual, 02090(1, 3) Lacquer color, by Gardner scale, D1544 (1,2,3) cellulose nitrate content, D3133(l) density and specific gravity, D35O50) definition of, 016(1,2,3) liquid/solid state, characterization, D4359(l) ester value, of lacquer solvents, D1617<3) $ a Burning characteristics freeze/thaw test, multicolored, D2337{1) guide for testing, D333(l) imprint resistance (of dried films), D2091O) partide size analysis(multicolored),D2338(l) Magnesium silicate * plasticizer migration, vinyl fabrics, 02199(1) analysis, D717(2) selection of test methods, D333(l) specification, 0605(2) stain removal ( multicolored lacquer) D2198(l) Sa Pigments, general properties temperature-change resistance, test, 01211(1) Maleic anhydride testing wood furniture lacquers, D2571(l) color, by platinum cobalt scale, D3366(3) viscosity by dip type viscosity cups, D4212(l) maleic acid content, 02930(3) viscosity by Ford viscosity cup, D1200(l) sampling and handling, practice, D3438(3) Lac resins See Shellac specification, 03504(3) Lampblack solvent extractable matter, test, D305(2) Mandrel bend test specification., D209(2) flexibility of organic coatings, 0522(1) Lampblack content, test, D305(2> Manganese content Lapis lazuli See Ultramarine blue of drier, 0564, 2375(2) Latex paints -- See Architectural paints of cellulose pulp, 04085(2) Latex vehicles Mar resistance filter-retained solids content, DS097(2) under development by D01.23 guides to test procedures, 04143(2) Marine coatings See Antifouling paints nonvolatile content, D4?58(2) Masonry exposure test panels, prep., 01734(1) unreacted monomer content, D4827,4747(2) Masonry treatments See Water repellents $a Emulsion vehicles MEHQ content Lead chromate pigments See Methyl ether of hydroquinone See Chrome yellow and orange Meier rods See Film applicators Chrome green MEK resistance Molybdate orange of ethyl silicate-zinc rich primer, D47520) Lead content, analysis Menhaden fish oil See Fatty oils air particulate filter samples, 04358(2) Mercuric oxide basic lead silico-chromate, D1844(2) analysis, 0284(2) leaded zinc oxide, test, 03280(2) specification, 0911(2) paint driers, D2374, 564(3)1 Mercury content red lead pigments, test, D49(2) in mercuric oxide, 0284(2) traffic marking material, D4797C1) in paint (low concentrations), 03264(1) white linseed oil paints, D215(l) Metal powder pigments yellow, orange, and green pigments, 0126(2) See Aluminum powder and paste Copper powder Lead pigments Gold bronze powder See White lead Zinc dust Lead chromate pigments Metal substrates, coatings on Basic lead silicochromate accelerated outdoor exposure, 04141(1) Red lead adhesion, by cut/tape test, 03359(1) Leaded zinc oxide blistering-evaluation of, D714C1) Lead silicochromate coil coatings, 03794(1) See Basic lead silicochromate ' flexibility/adhesion-deformed, 04145(1) Lead molybdate See Molybdate orange mandrel bend test, D522{1) Lead oxide See Red lead primers, testing practices, 03322(1) Leaded zinc oxide, analysis, 03280(2) Leafing properties aluminum powders /pastes, D480(2) Metamerism, visual evaluation, 04086(1) Leveling (ropiness) of paints, test, D4062(l) Methacrylic acid (glacial 95.5%) | specification, 03845(3) Methanol (methyl alcohol) acetone content of, D1612 (3) content, in formaldehyde solutions, D23 permanganate rime, test, 01363(3/ specification, D1152(3) Methoxyl content hydroxypropyl methylceUuiose, D236S1 methylcellulose, D1347(2) Methoxyl/hydroxypropyl substitution by Zeisel-gas chromatography, D3876(2) Methyl acrylate, specification, D4709(3) Methyl alcohol. See Methanol Methyl amyl acetate, D2635C3) Methyl amyl alcohol See Methyl isobutyl carbinol Methyl amyl ketone purity, by gas chromatography, 03893(3) Methyl butyl ketone purity, by gas chromatography, D3893<3) Methylcellulose See Cellulose and cellulose derivativi Methylcyclohexane purity from freezing point, test, D1016(3) Methyl esters, fatty acid composition, D1983 preparation from fatty adds;, D3457(3) preparation from oils, D280Q(3) Methyl ether of hydroquinone (MEHQ) coni of monmomeric acrylate esters, D3125(3) Methyl ethyl ketone 99.5% grade, spec., D3729(3) purity, by-gas chromatography, D2804(3) spec., D740(3) Methyl isoamyl ketone purity, by chromatography, D38?3(3) spec., D2635(3) Methyl isobuty! carbinol, spec., D2635(3) Methyl isobutyl ketone analysis by gas chromatography, D3329(3) spec.. Dll53(3) Methyl methacrylate unreacted monomer in latexes, D4827,4747(2) Methyl n-amyl ketone 98% grade, spec., D4360(3) Methylol group content in phenolic resins, test, D4706(2) Metric practice--SI Units, excerpts, E350(l, 2^ 3)| MFFT See Film formation, emulsion vehicles1 Mica pigment r analysis, D716(2) spec., D607(2) * - - Microbiological attack -See Biodeterioration Microcoulometry See Coulometry Micro-organism resistance See Biodeteribration Migration of plasticiser from vinyl fabrics to lacquers, test, D2199(l) MUliequivalency, acid/base See Electrocoat baths Milori blue See Iron blue Mineral (hydrocarbon) oils ?. moisture content, D890(3) content in rosin oil, D1131(3) Mineral spirits aromatic content, chromatography,D3257(3) specification, D235(3) Miniature sandtnill method color and strength of pigments, D3022(2) Minimum film formation temperature (MFFT) See Film formation, emulsion vehicles Miscibility lacquer solvents, with heptane, Dl476(3) water soluble solvents, with water, Dl722(3) Mixed aniline point dipentene/terpene solvents, test, D801(3) 1126 DUP050298303 Condensed Index of Committee D-1 Standards Figments--color categories S ee Blade pigments Blue pigments Brawn pigments Glass beads Inert pigments (Extenders) Meld powder pigments Nacreous pigments Orange pigments Red pigments White hiding pigments Yellow pigments Pigments--composition categories See Earth pigments Iron oxidepigments Lead chromate pigments Chromium pigments Pigments--function categories See Anti-corrosion pigments Anti-fouling pigments , Anti-fungal pigments ,, Colorant pigments Extender pigments (inerts) White hiding pigments Pigments--general properties bleeding characteristics, D279(2) composition acidity/alkalinity, Dl208(2) ignition loss Dl208(2) moisture content,D280, D1208C2) volatile content, D4139(2) water soluble salts.content, P2448(2) lightfastness in artist paints, D4303(l) oil absorption Gardner-Coleman method, D1483(2) Spatula, rub-up test, D281(2) . , particle size characteristics; reporting of, D1366(2) course particle content, D165(2)t fineness of dispersion paint, D1210(1) fineness of grind, printing ink, 01316(1): . particle size distribution, 03360(2) specific gravity, D153(2) tinting strength and color colored pigments -- with mechanical muller, D387(2) with miniature sand mill, 03022(2) white pigments-- visual method, D332(2) instrumental method, 02745(2) Pigments--in paints and dispersions See pispersion/ftnenessofgrind Lightfastness Pigment content Slurries White pigmentS/chemical analysis Pine oil moisture content, 0890(3) sampling/testing, 0802(3) Pine tar/pine tar oils sampling and testing, D856(3) pinholing film failures of exterior latex paints, D1848(l)l Plasticizer migration vinyl fabrics to lacquers, 02199(1) Plastics coatings for plastic substrates, D3002U) epoxy content, 01652(2) Platinum-cobalt solutions, color scale See Color Polyester resins See alkyds Polyhexafluoropylene (FEP) substrate for preparation of free films, 04708(1) Polyhydric alcohols content See Alkyds Polymeric powders/powder coatings test procedures, practices, 03431(1) Polymerization cellulose nitrate, test, 01716(2) dipentene/terpene solvents, test, D233(3) unreacted monomer of latexes, D4747(2) Polymerization inhibitors: : butylcatechol in styrene, 02120(3) Polymerization time. electrical insulatmg sheUac, D411U) Polymers silicons^ilicon content, 03733(2) solubility range, test, 03132(2) Polyurethanes See Urethanes Polyvinyl butyral resins See Resins--polyvinyl butyral Polyvinyl chloride (PVC), chlorine content, test, 01156(2) residual vinyl chloride, D3680U) test procedures, guide, 04368(2) Porosity, of paint films, D3258(l) Potashblue See Iron blue Powder coatings 5 ee Polymeric powders/po.wder coating Practices ( See individual standard practices.. S a Guides for testing Precision See Statistical methods Primers ethyl silicate - zinc rich MEEC resistance, cure test, 04752(1) formability on steel, ^04146(1,) test guide, on pre-jfbrmed metal, D3322(l) Primrose chrome/yellow See Chrome yel(ow and orange Print resistance oflacquers,02091(1) i of architectural coatings, in preparation Printed matter . evaluating lightfastness, D3424(l) Printing inks and vehicles apparent tack, inkometer test, D4361(l> fineness of grind, NIPIRI method, 01316(1) . lightfastness, printed matter, D3424(l) nonvolatile content, 04713(1) tinting strength, in prep, viscosity, by falling-rod, 04040(1) water pick-up, D4942(l) S a Resins, Resin solutions 1- Propanpl . See n-Propyl alcohol 2- Ptopanone See >. Acetone Propionyl content cellulose acetate propionates, 0817(2) Propyl acetate, normal alcohol content/purity, 03545(3) 90-92% grade, spec., D313O0) n-Propyl alcohol, specv 03622(3) Propyleneglycol monomethyl ether. PGME, purity, 04773(3) ; , spec., 4837(3)' Propylene glycol monomethyl ether acetate PGME acetate, purity, 04773(3) spec., 04835(3) Propylene glycol, spec., 02695(3) Prussian blue See Iron blue Pull-off strength (bond strength) See Adhesion/Cohesion Pull test, static friction, 04518(1) Pumice/pumice stone/pumacite specification, 0867(2} Purchasing, state/institutional, 03927(1) Rare earths content print driers, by EOTA method, I Raw oils (drying oils) See Fatty oils Raw aiemta/umber See Sienna, burntandraw Umber, bumtandraw Reagent water ^ microelectronic processing, spwc 1)1193(3). reagent water, spec., 01193(3) \ J *, Red copper oxide (77402) See. Cuprous rude ^ Rediron oxide Red lead - See Iron 4 red analysis, 049(2) specification, D63<2) .. *0* -j:,; $a Pigments, gsneraL.pi^ptfriw 'v Red oxide of mercury See Mercuric sonde Red pigments See Iron oxide red (synlhetir/naiunt) Para (paranitranilinc) red. ^ ` '* .,^1 Red lead , ' Toluidine red (> Venetian red Reflectance and reflectivity . V gray scale, evaluating color riunge, T>261GU> r hiding power by reflectometiv, D2BQ5CI) '* {,, instrumental color difference, 02244(11 "* *vMunsell color system, D1535(1) ,, o&JPfMHlI of opaque spedmens,.E97(l) , preparation of reflectance sta* d. I specific luminance, traffic coaLng-, t>JUGl(rfL)'V'w Refiective markers in traffic p.iint ^ > * ,, See Class beads 7i( Refractive index frt \ dipentene/terpenes, D801(3) pine oil (rtatural/synthetic), D8p2(3)`/ turpentine and pinene,:test> DS33(3) Repellents, See Water repellents - ^ Reporting paint film failures of exterior latex paints; 1)1(548(1/ Reproducibility and Repeatability See Statistical methods $ \ j jj Resin solutions,general properlitj clarity/cleanness, D?090{1,3) ^ ,3 cloud point, D5G62(3) * dilutability (solvent toleranoJ, USUfJtsl Gardner color scale, b-1544(l,2^5) anonvolatile, ink vehides,i>4713U' < nonvolatile matter content, <te t, 1>12WiZVj std. color solutions, D365(2), Dl209(^^g unsaponifiable matter, D1397<2) | viscosity, test, 01725(2) . v Resins,general properties - *! softening, ring and ball, E28(3) ,f solubility/range, test, D3132(2) . volatile/nonvolatile, .1)4209(2) volatile resin acids, 03008(3) water content, Karl Fischer, b -1 P'y1~TI Resins, various types > * * .. A' See Alkyd resins Amino resins '.49 Epoxy resins Phenolic resins. Rosin Shellac (lac) Urethanes Vinyl resins Rockr . spa**., >Ro1k!* I 1128 DUP0502 98304 Condensed Index of Committee 0-1 Standards Instance properties/resistance to Rosin ^ See Abrasion resistance add number, 0465(3) Acidresistance ash; burning residue 4 Alcohol resistance iron content, D1064(3) Alkali resistance : ' sampling and grading, 0509(3) Bleeding4 saponificadon number,0454(3) B ^deterioration tall oil rosin-fatty acids,: 01585(3) > Blistering unsaponifiable inatter,pl065t3) toluene insolubles,D2693(3) volatile oil content, 0889(3) Chemical resistance volatile resin acids content, D3Q0B(3) Chip (chipping) resistance Rosin acid content Coffee stains coating vehicles;- 02439(2) Corrosion resistance fatty adds, test, D1240(3) Cracking (crack resistance) rosin oil, test, D1131(3) Detergent resistance tall oil, test, ;D803(3) Discoloration lac resins, test, D29(2) Erosion resistance Lieberman-Storch test, 01542(1,2) Exposure (weathering) Rosin esters . . Flaking rosin adds content, 01469(2) Fuel oil/resistance r; . Rosin oils, testing of> D1131(3) Fvmgus.tesiStanee Rouge 5 ee Iron oxide red Gas cocking ... Rub-out test (pigments) Gasdttae resistance See Ott absorption (pigments) Heat resistance Rusting-degree-photographic standards Household chemicals bn painted steel Surfaces, D610(l> v Humidity resistance Impact resistance Lighfresistance Mar resistance . Safflower oil ? Microbiological attack : . specification, D.1392{3) Microorganisms Sa Fatty oils Mold resistance Sag resistance test Mortar resistance Using a muidnotch appUcator, 04400(1) Oil resistance Salt spray (fog), resistance Oyer baking Perspiration resistance with acetic acid,'B287, 117(1) Sampling Print resistance liquid paintsdepigmented coatings, D3925{1) Sag/sagging resistance Sand abrasion test Salt spray resistance falling sand method), 0968(1) Scratch See Mar resistance Sandstone, architectural Scrub resistance preparatory surface cleaning, 05107(0 Slip resistance Saponification number/value * Soil/dirt resistance drying oils, fatty adds, D1962(3); Soiventresistance . lac resins, test, 029(2) Spattering (spatter resistance) rosin, test, 0444(3) Stein resistance tall oil, test, D803(3) Water resistance S a Unsaponifiable matter content Wear resistance Saybolt viscometer See Viscosity Wet abrasion (scrub) resistance Scaling See Flaking Scattering coefficient; absolute values (hiding power), 02805(1) pRetroreflecfion (horizontal coatings) white pigments, relative values, D2745(2) ! traffic paints, specific luminance, D406K1) Scratch resistance See ' , Mar reeistance (theological properfiea/rton-Newfconiart coatings] Scrub (wet abrasion) resistance Brookfield viscometer, D2196(lh See Wet abrasion (scrub)resistance ICI cone/plate viscometer, D4287(l) S a Viscometers (viscosity) Sealants Sec Caulking/glazing compounds Ring-and-ball apparatus Sealers (floor) f softening point, of resins, E28{3) See Floor paints/coatings Hoad service testing See Traffic paint Semi-gloss paints See Architectural paints Sericite See Mica Rocker hardness test(Sward) See Hardness Setaflash tester Roller application, of paint See Burning Characteristics Settling .,. ! hiding power,praefical, D5150(l) traffic paint, accelerated, 01309 spatter resistance, D4?07(l) traffic paint, in containers, D869(l) |Rollers, paint See Paint rollers, covers Set-to-touch-tim e See Drying properties Ropiness (of paints). See leveling Sheen See Gloss and Sheen Sheet metal (with organic coating) Rosenimmd-Kuhnhenn method flexibility/adhesion of the coating, 04145(1) iodine value of drying oils, 01541(3) mandrel bend test, D522(l) Shellac (lac resin) bleached shdlac spec., 0207(2) copal resin content, 029(2) for electrical insulation, 0411,784(2) orange shellac and other lacs, spec., D237(2) sampling and testing, 029(2) shellac varnishes sampling and testing, 01650(2) specification, 0360(2) volatf]e/non-volatile content, 04209(2) SI units (Intemational System of Units) metric practice, excerpts, E380,(l,2,3) Sienna (bumtand raw) analysis, 050(2) ^specification, 0765(2) , Sa Pigments, general properties . Sieve analysis glass spheres, used in traffic paint, 01214(2) pigments, practice for reporting, 01366(2) pigments and dispersions, (0185(2) Silanes, siloxanes See Water repellents Silica, diatomaceous analysis, 0719(2) specification, D604(2) Silicate pigments See Aluminum silicate Calcium borosilicate Calcium silicate Magnesium silicate Silicone-coated paper preparation of free films, 04708(1) Silicone polymers silicon content by spectrophotometry, 03733 Skinning See Stability--package Slip resistance; static friction test 02518(1) Slurries titanium dioxide content, 03926(2) Soapstone- See Magnesium silicate Softening point organic coatings, test, 02134(1) resins, ring and ball apparatus, E2S(3) Soil accumulation, on paint films degree of surface disfigurement, D3274<I) Soil/dirt resistance (removal) practical washability, 04828(1) Solid/Liquid state, characterization, 04359(1) Solids content ...__ * See - Nonvolatile/volatile content Solubility tests cellulose in sodium hydroxide, D1696(2) cellulose nitrate, D301(2) solubility range (resins/poiymers), 03132(2) Solvents See Solvents-chcmical types Solvent resistance Solvents, test procedures, general SoJvents-chemical types See Acetate ester solvents Alcohol solvents Aliphatic hydrocarbon solvents Aromatic hydrocarbon solvents Ester solvents Glycols Glycol ether acetates Glycol ethers (ether-alcohols) Halogenated solvents Hydrocarbon solvents Ketone solvents Terpene solvents 1129 DUP050298305 Condensed Index of Committee 0-1 Standards Solvent resistance alcohol, on furniture lacquer/ D257t(l) gasoline/fuel cal, on traffic paint, 02792(1) MEK, of ethyl silicate primer 04752(1) Solvents-test procedures/general analysis, chromotography, 03271(1) clarity/cleanness, 02090(1,3) Stpel surfaces, unpainted pictorial standards of condition, 02200(1) profile of abrasive - cleaned steel, 04417(1) test panels, preparation of, 0609(1) - >' Steel surfaces, painted - See Exposure, accelerated Exposure, exterior > Texture f gloss differences of similar -.( ' ( ( ,, UiJwni.'ft Therraalvoltaic infrared ihennoir^ ters * See Infra-red pyrotnetry' * Thermistor infrared radiation tfr-vromitim See Infra-red pyrometry Thermosetting resins evaporation rate, D3539 halogenated, in paints, analysis/ 04437(1) hydrocarbon solvents acidity, test, 01613(3) aniline point, 0611(3) benzene content, D4367(3) Kauri-butanol test, 01133(3) Stiffness of free U.ms,O2370(l) Stormer viscosity(consistency) - ! of paint 0562(1) - of pine tars-and pine taroils, D856(3) Strip (copper tarnish) test stroke cure timeof phemlics, 04640(2)* **K& Tpickness--paints/related coatbigs ,. . y producing ttniform films, 0823(1 1 Set Film thickness measurement Thinners See Mineral spirits, Turuentun. `copper corrosion in petrcleuahproducts*, Dl30(3)j Stroke cure time '> : ; = ; VM &P Naphtha ' ). Sa Solvents?- ,,, , Ip odor (characterstic/residuaL), 01296(3) thermosetting phenolic resins, D4640{2) - Thixotropy sampling/test procedures, D268(3) Strontium chromate, analysis/ D1S4S(2)* l: water content, by Fischer reagent, D1365(3) ' Sa Pigments, generalproperties -- rotational (Brookfield^viscOou t r, 02190(1) Sa Viscometers , 4,5HI identification in point, 02349(1) Structural coatings Tinting strength , Vt lacquer solventS,heptane miscibility, D1476(3)[ field identification/analysis, 05043(1) chromatic pamts, 04838(l) f water miscibility, 01722(3) Solvent tolerance See Resin solutions ' Soybean oil -degummod/spedfication, 0124(3) 'refined, specification, 01462(3) Sulfide content -v - . white pigment, frortfpajhf/02352(2) Sulfurcontent l- * * ' cellulose materials, 02929(2) < white pigm6n^frompaiiit,D2352(2)- Sunfloweroil ' * . 'printing inks, in prep. t i white pigments, mstrumextfab 02715(2) j. white pigments, visual^ 0332(2) > colored prigments, 0387,3022(2) 5a Pigments, general properl t>s Titanmm dioxide Sa Fatty oils ' specification, 03169(3) SaFatty^oilS ^ Fatty acid teste, specifications Surface analysis Spattering (spatter resistance) adhesion, tests, 04541(1) 'analysis of and for ( anatase/rutil&ratio, 0372Oj(2)i I atomic absorption spectroscopv, p AhSlCllg roller application test, 04707(1) Spatula rub-out test ' . gloss differences, visual evaluation, 04449(1) \ by X-ray spectroscopyi.^Hiu.s ,W ' gloss goniophotometer, 430(1) u- r = chemical analysis, D1394<2> . ^ See Oil absorption, pigments /profile, blast cleaned steel, B44l7(l>`r w- ! in traffic markuig paiat,:B4r')7(l)# ' Specific gravity static friction, D4518(l) ?t^ * - slurry-solids content, D3926(;> of pigments, 0153(2) Surface preparation--for paintuig?* "> specification, D476(2) Specific luminance, horizbntal coating abradingof concrete; 04259(1) *: tinting strength, instrumental; D-/45'Z1 traffic stripe paint, 04C61O) add etching of concrete, 04260(1) r :i 'tinting strength, visual, Specific permeability aluminum (hot-dip); 01731(d); >. S a Pigments, general proper ties ' See Moisture vapor permeability : aluminum/aluminum-alloy surfaces, 01730(1) Titer Spectroscopic analysis ' \ architectural sandstone, 05107(1) ! ` - r fatty adds, test, 01982(3) acryfic^jpdlynler in emulsioh ^amt/ 03168(1) ' concrete/masonry panels, D1734U)' >'* Toluene antimony content (low cone), D3717(l) ' ; galvanized steel; non-passivated, D2201(l) - industrial grade, spec, .0 11 *1 cellulose nitrate lnalkyd lacquers, 03133(1) glass panels, D389K0 ; ; toluene insolubles irUrosm;D269(al j dhrornium content(ISiv cone), 03718(1) ` : ! ' diene value, dehydrated castor oil, D1358(3) magnesium-alloys, 01732(1) steel test panels, 0609(1) - volume and weight calcination 113." Toiuidine red identifying separated vehicle solids, D2621(1)J Sustained burning test ' analysis, 0970(2) . iron content (of rosin),01064(3) Seta-flash tester (open cup), 04206(3)- specification, 0656(2):- ; lead/cadmium/cobalt, 03335(1) 1 Wick test,04207(3) '* ' Took gago>-' s Fiini'thickness? uiv lead/chromium in pigment dust, 04358(2) lead content in pauit, 04834(1) Sward rocker See Hardness testing ' 1n mercury contentdoiv concentration), 03624(1) Traffic paint : \ metal content of cellulose pulp, 04085(2) Taber abraser test. See Abrasion resistance \ adulteration of vehicle sohdfi->02^aari^j^p siilfur content of Celhilbsics, 02929(2) '* Tack, of printing uiks,Inkometer;04361il) bleeding, over tar and asphalt titanium dioxide in paint, 04563,4764(0 Tag cup See ' Burning Characteristics ; bleeding, photographic standards 0^' iH * * traffic paint vehicle adulteration, 02743(1) Talc See Magnesiumsilicate'- 1 conductingtqgdaemoe tests, D713I0.1 Specular gloss See Glossand Sheent Tall oil/ test methods for, D803 ; degreedf <5upping> 0913(1) Spoilage See Biodeteriorafibn : Sa Fatty oils degree ofsettlmg,869(1) ^ Package stability Tall oil rosiri glass spheres, tbiiridiifes;03jl55(2) m a-'Vi Spray application < Fatty acids--tests, specifications' - l glass sphefes/.'sieve ana1ysis>>T)12T4(2>, See Transfer efficiency " - Tall oil rosin - fuel c*il/solvenfresistaijce^.027y2tl> Spreading rate fatty acids content, 01585(3) gasoline resistance, D2792(l)i . hiding power of paints, 0344, 2805(1) volatile resin adds content, 03008(3) 1 no-pick-up (drying) time, D7U.0 -.at ^ i Stability--package See Package stability , pigment content,' by ashing, D4451(1)-:^ Stain resistance practices for testing, 02205(1) coffee stains, 0 2571 (1) Tar See Pine tar/pine-tar oils : retroreflectance/spedfic luminaiUL: vm of factory applied wood fini$hes,.03O23(l) Temperature tests settling dufingstorage, 01309(0 1 ofmulticolor lacquers, 02198(1) freeze-thaw resistance, 02243(1) wear life/resistance, D913(l) of organic finishes; 01308(1) , low-temperatuxe coalescence, 03793(1) Transfer efficiency-sprayapplical lorn j of transportation industry finishes, 01540(1) minimum film foririadoti temp. D2345<?) under laboratory conditions, 05009(1); of wood furniture lacquer, D2571(l) Tensile properties; of free films, 02370(1) under production conditions, DSCO&U) \ Sa Wa.shability, Porosity Terpene solvents Tribasic lead phosphoSiltcate : * >4vq Static friction tests (slip resistance) See Dipentene/PineOil, Turpentine analysis, 02742(2) inclined plane/horizontal pull, 04518(1) Terra alba See Caitium sulfate specification 02744(2) ... - ' J'-4$ Statistical methods Terra de sienna See Sienna (burnt and ravV) Tributyltin See Organotint for interlaboratory testing, E691(3), 03980(1) Test results Ste Forms fdr recording Trichloroethane determination Steel blue pigment See Iron blue Testing, interlaboratory practice, 03980(0 by gas chromatography;:D4457`(j) 1130 ?**#&*& DUP050298306 Condensed Ifidfe* ot Comnittpc 0 1 Stahdar.ds Tricresylphosphate permanganate time, D1721(3 . specification, 0363(3) unsaponifiable matter Content, 01399(3) volatile matter content>T>1468{3) Tristimulus values See Color - opaque materials Tung Oil gel time, test, D1955(3) quality determination, Dl964l3).v. - raw, spedficatioiF/p.l2.(3> \ ^: *': Tunnel method(two>foo6tunne]} : h fire retardancy of paints, D3806(l) wflh -r Turkey red See Iron oxiefered ,wr Turkish umber See Umber(biimt andifaw) Turpentine .' < :r ;* pinene composition, D3009(3).. r. v. sampling and testmg>'D233(3) c' - * x spedfication,.Dl3(3)-' u.`o- Two-foot tunnel method fire retardancy of paints, 03806(1) Ultramarine blue analj^sis, 01135(2) specification, D262(2) Uitraviolet-cured coatings cure time, reporting of, 03732(1) package stability, D4144(l) Ultraviolet exposure, D4587(I) Umber (burnt and raw) analysis, D50(2) specification, D763(2) Units, SI, metric, 380(1,2,3) Unsaturation (in drying oils and derivatives) Rosenmund-Kuhnhenn method, D1541(3) Wijs method, 01959(3) Urea-formaldehyde resin solutions See Amino resins Urethanes free toluene diisocyanate content, D3432(2) 2-ethoxethyl acetate in, spec., D3728(3) isocyanate group content, D2572(2) isocyanate raw materials, 01638(3) methyl ethyl ketone in, spec., D3729(3) UV See Ultraviolet-cured coatings . Ultraviolet exposure Vanadium content paint driers, EDTA method, 03988(3) Varnishes abrasion resistance: air .blast, D658(l) falling sand method, D968(l) acid value, test, D1639(l) , acrylic add, spec., D4416(3) bleached lac varnish, testing, 01650(2) clarity/cleanness, visual, 02090(1,3) def. of terms, D16(l, 2,3) density, test, 01475(1) discoloration (light stability), 02620(1) household chemicals, effect, D1308(l) elasticity or toughness, D1642(1) elongation/tensile strength, 02370(1) exterior durability, test, D164K1) drying at room temperature, 01640(1) flash point, test, D3278(3) Gardner color scale, 01544(1,2,3) gas checking and draft test, 01643(1) humidity resistance, 02247(1) indentation hardness, test, 01474(1) moisture vapor permeability, 01653(1) nonvolatile matter content, D1644(l) preparation of free films, 04708(1) preparing glass panels for testing, 03891(1) Varnishes {continued) t u, , preparing ,tc I finds for t< emp, TVOOfcO-i, ; irosinada,uontert 131469(2) * - ; rosin content I i nrrum StUiJi,, m$42ll,2> \ rosin content, Halphen-Hicks, 01342/1, 2) scrape adhesion test, 02197(1) selectibfif'oftest procedures, D154(1),- i shellac vand5jfr^?testiag,Dl6S0(2) specific gravity at 25/25C, D1963(3) test environments, D3924(lX, s viscosity, dip-type viscosity cups, 04212(1) viscosity. Ford cup, 01200(1) volatile/nonvolatile content, 04209(2) water and^alkaliresistance^ 01647(1) water immersion test,U870(l) weathering tests onwood, 0358(1'). i ) wet film thickness, D1212, 4414(1) Vehicles, solvent type^pigmented.. . . i centrifuge for pigxnentCorrtenti':D2371,2698(1) : centrifuge for vehicle separation, D2372<1) j non-volatilecontent,pi%tinginfcs5;04713 \ i solids identiiication, 'infra>rcd, D262l(l)! Venetian red, analysis, D50(2);1 .r ^ ; Sa Pigments/general properties1 Vinyl acetate a*.: .. acetaldehyde content, D2191(3) l acidity, test, 02086(3) - :>< - , hydroquinofiecgntentr, D2193(3) , < 1 specification, O2$90(3)?m:^ ^ Vinyl chloride nibndmerrfiresidiial) content , x j in polyvinyl chloride resins ; - * yinyliesins 'h > polyvinylbutyral,01S96<2); . <* = polyvinyl chlorid6;,0436fi(2hv, v Viscometers (viscosity) : i.; . ' bail drop niethodrcellulose, 01343(2) Brookfield (rotational), 02196(1) . bubble time,.dear liquids, 01545(1,2,3) dip type viscosity cups, D4212(l) falling rod (printing inks/vehicles), 04040(1) Ford cups (paints/varnishes), 01200(1) Gardner-Holdt, D803(3) [Cl cone/plate (high shear), D4287(l) ISO flow cups, 05125(1) Saybolt, D856(3) Storms (Krebs units), 0856(3) Weissenberg, rheogoniometer, 03451(1) Zahn cups (coil coatings), 03794(1) VM & P Naphtha specification, D3735(3) VOC (Volatile organic compounds) paints and related coatings, 03960(1) automotive coatings, abatement, 05087(1) Volatile liquids rate of evaporation, D3539(l) Sa Solvents Volatile matter content See NonvolatUe/volatile content Volatile organic compounds (VOO, 03960(1) Wick test (low viscosity mixtures), D4207(3) Washability, of architectural paints soilant - mechanical washing, 03450(1) stains & soilants - practical test, D 4828(1) Sa Wet abrasion (scrub) resistance Water--high-purity/reagent-grade reagent water, spec., D1193(3) Water-borne paints See Architectural paints Artists' paints Industrial finishes Water colors See Artists'paints \Wer cuirienl--paints'relnied i t* In {M* uiirytit4U>TiJpJiV, Od79i(* I n d xu* ret gm* nnuach 016310; , cri Ji crta^K . id, DMA (3) fx uliUj i (.nmpttiui-K, D2Us2<3) in dir D4287U) ' Kgrl Iisehcri*ietifc uicthod, U40r<l) Liquid t o \ 1 s I/> 0*, O490(V' P* tt > ! um products l / d^Latwn, 09313, ) I1 W pigment p O I20R(2) solvents, byiRj^Hirr^ puit nuhod OilMO) terpene solvent > Ob1"' Water fog test. Organic coatings, 01735(1) ' Water immersiontest , : paints i m^tol Ofc7U(l) Water miscibility See Miscibility Water pickup test . : ? ............ v. See Printing Inks ,, Water-reducible coatings industrial type, testing guide, 04712(1) Water repellents * for wood; evaluation of, D---;(l)-m prep, masonry treatments,silane,non vol,D509S(l) qualitative test for in wood; 02921(1) .. Water resistance of coatings boiling water, of furniture lacquer, D2571(l> , controlled condensation, 04585(1),' \ of varnishes; 01647(1) , waler-fog test, 01735(1) * wa immersion test; 0870(1) ` 4 1 rSa Humidity resistance .%,, Water-soluble matter, content drypigmfentfe, 01208,2448(2) lac resins> D29(2) . -t pigments (lead chromate type), 0126(2) salt content, biue-pigments, 01135(2) salt content of pigments, 02448(2) Water spotting,exterior latex paints,01848(1) Water vapor permeability, 01653(1) Wear resistance (Wear life) of traffic paint, D913(l) 5a Abrasion resistance Weathering See Exposure Weatheroineter, See Exposure-accelerated Weissenberg rheogoniometer test viscosity of powder coatings, 03451(1) Wet abrasion (scrub) resistance scrub-to-failure method, D2486(l) > - -- weight loss method, P4213(l) Wet film' thickness gages See Film thickness gages, wet film Wet ground muscovite mica See Mica Wet-to-dry hiding change of paints, D5QG9(1) White architectural enamels See Architectural paints and coatings White extender pigments See Extender pigments White hiding pigments See Antimony oxide Basic carbonate of white lead Basic sulfate white lead Titanium dioxide Zinc oxide Zinc sulfide Sa White pigments, chemical analysis Pigments, general properties White lead See Basic carbonate of white lead Basic sulfate of white lead *j U3I DUP050298307 Condensed Index of Committee 0-1 Standards Si White pigments, analysis extracted from paint antimony oxide content 02350 combined sulfur, D2351,02352(02) general, 0215 (01) practices and methods, list, D34(02) S a White hiding pigments Extender pigments White zinc See Zincoxide Whiting! See Calcium carbonate Wick test See Burning Characteristics Wijs procedure--iodine value drying oils and derivatives, D1959(3) fatty amines/diamines, test, D2075(3) Wire-wound drawdown bar (Meierrod) coating application method, 04147(1) Wolfe-potenriometric method fatty acids in tall oil rosin, 01585(3) Woad chlorinated phenol in, test for, 02921(1) exposure tests on wood, 01006(1) panels for weathering tests, 0358(1) Water repellents for, under deveL by D01.42 ^vvater repellents in, test for, 132921(1) Wood finishes blocking test, 02793(1) dry him thickness, D2691(l) exposure tests, practices, D1006(l> factory applied: liquid/fresh film, properties, 02336(1) factory primed, durability tests, 02630(1) humid-dry cycling, 03459(1) preservative, chlorinated phenol, D2921(l) temperature of coating cure cycle, 03259(1) weathering tests, panels for, 0358(1) Sa Factory applied finishes Wood rosin. See Rosin Wood sash glazingcompounds See Caulking/glazing/sealant compounds Wood turpentine. See Turpentine Xenon lamps exposure, nonmetaUic materials,, G26(l) lightfastness of pigments, 04303(1) Xylene ten-degree, spec,D346(3) Zinc drier, p, Zinc dustpigment analysis, 0Sil(2) Specification 1)520(2) Zinc hydroxy phosphite mm. analysis, EMfsOte) specification, DS462(2) Zinc oxide analysis, D3280(a) specification, D79(2) mm Yellow ocher See Ocher Yellow pigments See Basic lead silicochroxnate - Chrome yellow Iron oxide yellow Ocher . Strontium chromate Zinc chromate Sa Pigments, peneralp Zinc-rich primer, Sea " Zinc sulfide analysis, D32W(2) -V'P & "fj specification DJ77(J) , yApJtyf Sa Pigments,general priuperlie' Zinc white See Zinctd Zincyellow ee Zinc cl Zirconium drier, Sr Driers Zahn viscometers Viscometers Zeisel technique, chromatography, ethoxy! substitution, 04794(2) methoxyl hydroxyprbpyl sub.,, 03876(2)^ Zincchromate analysis, 0444(2) ` specification, 0478(2) 5a Pigments,generalproperties Ziztc-coated (galvanized) surfaces preparation for painting, 02092(1) Zinc content driers, EDTA method, 02613(3) white linseed oil paints, 0215(1) white zinc pigments, 032800) zinc dust pigment, 0521(2) zinc hydroxy phosphite, 04450(2) `jfe!- 1132 SiiU.i; DUP0502 98308 ANNUAL BOOK 1E ASTM STANDARDS Index Section 6 PAINTS, RELATED COATINGS, AND AROMATICS This index.covers the standardsfand related material appearing in Volumes 06.01, 06.02, arid 06.03. The boldface references are to the iSTM designations; the standards appear in each volume in alphanumeric order. Proposed methods atib specifications'carrythe index bference, "(Proposed)"; they appear, as does other ancillary material, in the Related Material (gray-edged) section in the back of the book. h triangle (A),preceding the. ASTM designation .denotes thatAdjunct Material for the standard is prihlshed separately; the Adjunct No. is |iven in the standard. A Combined Index, covering.the standards appearing in all volumes ofthe 199-2 Akntial B6ok ofASTM Standards, is issued as Volume 00.01. ' ...... S Alphabetization in the index is letter-for-letter, with no consideration to punctuation or word division. Initial prepositions of (indented) iubentries are ignored for alphabetization. In the preparation of indexes, every attempt has been made to index standards on three levels; (1) by main subject, using general and Specific search terms; (2) by test methods or other significant sections ofASTM standards; and (3) by crossrrefeiences to locate-main subject bntry terms.'(Sie also refeibnces ^re'abbreviated as'Shrind appear under main entry terms.) Specification E451, for Acrylic Bone Cements (Volume 13.01), illustrates ASTM's method of indexing. INDEX TERMS FOR MAIN SUBJECT ENTRY :, Adhesives--4hbgifctil implant materials ' acfyllc bohe cements (for internal orthopedic prostheses), self-curing, spec., F 451 '".... . Orthopaedic medical devices---bone acrylic bone cements (for internal orthopedic prostheses), ; self-curing,, spec., F4S1 INDEX TIjRMS FOR TESTS Compressive strength acrylic bone cements, test, F 451 Doughihg time acrylic bone cements, test, F 451 CROSS-REFERENCES; Bone--cement See Adhesives--surgical implant materials Fixation materials .! -- Sa Orthopaedic medical devices (headings) DUP0502 98309 Index of ASTM Standards, Section 6 A Ablative antifouling paint systems See Antifonling coating system Abrading abrading concrete, practice, D 4259 (06.01) Abrasion resistance abrasion resistance of organic coatings, by failing abrasive, test, D 968 (06.01) abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) air blast abrasion tester, A D 658 (06.01) scrub-to-failure of interior latex flat wall paints, test, D 2486 (06.01) Taber abraser, test, D 4060 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) Abrasivcs/abrasivity conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) profile of abrasive blast-cleaned steel surfaces, in laboratory/ f field/fabricating shop, test, D 4417 (06.01) resistance of steel pipeline coatings to abrasion, by slurry of coarse abrasive/water, test, G 6 (06.01) Absorption gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) ,` Absorption spectroscopy lead content in paint, bydirect aspiration atomic absorption spectroscopy, test, 1) 4834 (06.01) Absorptive coatings relative tinting strength of chromatic paints, test,.D 4838 (06.01) Accelerated testing--paints/related coatings/materials accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame, carbon-arc light/water exposure apparatus, practice, D 822 (06.01) coatings (apptied to metal substrates), practice, D 4141 (06.01) edge performance of composite wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D 1654 (06.01) nonvolatile content of latexes, test, 11,4758 (06,02) wet abrasion resistance of interior paints to scnibbirig, by weight loss, test, D 4213 (06.01) wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Accelerated testing--pipeline ceatings cathodic disbonding of pipeline coatings, accelerated procedure, - test, G 8 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G 17 (06.01) resistance of steel pipeline coatings to abrasion, by slurry of coarse abrasive/water, test, G 6 (06.01) Accelerated testing--salt spray (fog) testing salt spray (fog) testing, method, B 117 (06.01) Accelerated testing--wood products wood used as panels in weathering tests of coatings, spec., D358 (06.01) Acetaldehyde (AA) Sa Aldehydes acetaldehyde content of vinyl acetate, test, D 2191 (06.03) acetaldehyde, spec., D4710 (06.03) acidity in vinyl acetate and acetaldehyde, test, D 2086 (06.03) Acetate esters alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) Acetic acid content cellulose acetate, test, D 871 (06.02) Acetic add (glacial) formic acid in glacial acetic acid, test, D 3546 (06.03) glacial (99.8 %) acetic acid (for use in pllUt IIsl lacquer/related products), spec., D 3620 (06.lJfl) Acetone ' ' acetone in methanol (methyl alcohol), t-st D lf,i i mn acetone, spec., D 329 (06.03) '^ acetone tolerance of heat-bodied drying oils tirf D 1950 (06.03) '. alkalinity in acetone, test, D1614 (06.03) apparent pH of water insoluble phenoI-MrmildchwV D 4613 (06.02) > permanganate time of acetone/methanol te-,t D 136.3 rtlg'f Acetophenone " "> analysis of major organic impurities in phenol prednd cumene process, by gas chromatogtaphv w D 4961 (06.03) Acetyl content acetone in methanol (methyl alcohol), t< st, I> 16121 apparent acetyl content of cellulose aceta e prnpnc butyrate, test, A D 817 (06.02) combined acetyl/acetic add content of cellulose at t <' 0 871 (06.02) Acetylene black See CarSon black {headings) SI Acid content acid/base milliequivalent content of(anome/cathouii ),> ', electrocoat baths/their ultrafiltrates, ta>t D 437<^mfll Acid-insoluble extenders j. .Sf' acid-insoluble extenders in (iron/copper phlhalocvumoeV' ultramarine) blue pigments, test, 0 1135 (06.02)' it? Acidity, alkalinity, pH--paints/related coalings/iimrurials acetaldehyde,' spec., D 4710 (06,03) _ _ * acid/amine value of fatty quaternary ammumurr cMor D 2081 (p6".03) . acid/base milliequivglent content of (ant dec uliodic). ,,, electrocoat batKs/their ultrafiltrates, u >t, 13 43"'0 (W^ acidity in vinyl acetate and acetaldehyde I s', U 2086 (0641 acidity in volatile solvents/chemical intermediates (USl-'J'ire paint/varmsh/lacquer/reiated products), test, D1613 (06.03) acidity of benzene/toluene/xylenes/solvert , i,l-d ,snmd4i,7 industrial aromatic hydrocarbons, t< st, D 8J" nt> 031 ,! alkalinity in acetone, test, D1614 (06.03) apparent pH of electrocoat baths, test, D 4584 106.011 apparent pH of water insoluble phenol-fi >-mjldch.dc < 04613(06.02) ', cellulose acetate propionates/butyrate, test, A DXI" >U6iii;' cellulose acetate, test, 0 871 (06.02) ' ethylcellulose, test, D 914-(06,02) formaldehyde solutions, test, D 2379 (06.03) hydrogen sulfide/sulfur dioxide (qualititative) of inoustral aromatic hydrocarbons, test, D 2363 (06.02) methyl acrylate, spec., D 4709 (06.03) methylcellulose, test, 0 1347 (06.02) moisture content of pigments, D 1208 (06.02) pH of chemically cleaned/etched concrete surfaces, D 4262 (06.01) Acidity, alkalinity, pH--plastics cellulose acetate propionates/butyrate, test, A 0 817 (06.02) Add number Sa Saponification number/value rosin oil, test, 0 1131 (06.03) rosin, test, 0 465 (06.03) sampling and testing pine tars/pine-tar oils, method, D856 (06.03) sampling and testing turpentine, method, D 233 (06.03) tall oil, methods of testing, D 803 (06.03) Acid phthalic anhydride See Phthalic anhydride 1134 DUP050298310 Index of ASTM Standards, Section 6 Aikyds/alkyd resins resistance '^/mortar resistance of factory-applied clear coatings on extruded aluminum products, test, 03260 (06,01) jluble extenders soluble extenders in (iron/copper phtlialocyanine/ ultramarine) blue pigments, test, D1135 (06.02) lue ' ./amine value of fatty quaternary ammonium chlorides, test, 0 2076(06.03) Hsvalueof organic coating materials, test, 0 163? (06.01) 1:y acids and polymerized fatty acids, test, D1980 (06.03) ipling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, D 29 (06.02) ish color uttatic hydtocarbons/related chemicals, terminology, 04790 (06103) esters V by gas chromatography, test, 0 3362 (06.03) lie add 'lie acid dimer in acrylic acid/unsaturated organic acids, test, D 4415 (06.03) icial acrylic acid (99.0 % grade),' spec., D 4416 (06.03) die latex paints Sa Latex paints fists' acrylic emulsion paints, spec., D 5098,(06.01) sts' paints (oii/resin-oil/alkyd), spec., D 4302 (06,.01) ieparing drawdowns of artists' paste paints; practice, i 04941(06.01) rater content of water-reducible paints, by direct; injection into | gas chromatograph, test, 0 3792 (06.01) Ik polymer content Ihlitative Identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, 03168 (06.01) we oxygen content--organic solvents ice peroxides (a5-80 ppm), using spectrophotometer, test, F.299(06:03) lesion--paints/related coatings/materials . inhesion of coating films to metallic substrates, by tape'test, 0 3359 (06.01) fhesioti of organic coatings to plastic substrates, by direct tensile testing, 05179 (06.01) jlear/pigmented organic coatings, test, D1308 (06.01) ^valuation of painted/coated specimens subjected to corrosive environments, method, 0 1654 (06.01) mar resistance of organic coatings, using balanced beam scrape adhesion add mar test, D 5178 (06.01) '' irganic coatings on prepainted deformed metallic sheets, test, D4145 (06.01) ipull-off strength of coatings, using portable adhesion testers, test, 04541 (06.01) by scrape test, 0 2197 (06.01) :inc-rich primer/chromate complex coatings (on steel), test, D4146 (06.01) hesive bonding bond strength of thermoplastic traffic marking materials, using cement bricks/sleel cubes, test, D 4796 (06.01) Ijihesives amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, 04948(06.01) ' commercial hexanes, spec., 0 1836 (06.03) Ihesives--structural trace peroxides (5-80 ppm), using spectrophotometer, test, E 299 (06.03) Ihilteration See Purity frican ocher See Ocher Aged coatings assessing the condition of aged coatings on steel surfaces, guide, 0 5065 (06.01) Aggregate impact resistance of pipeline coatings, by limestone drop test; G13 (06.01) Air blast abrasion tester paints and related coatings, test, A D 658 (06.01) Air blast cleaning oil/water presence in compressed air (used for coating application/air blast cleaning/abrasive blast cleaning), 0 4285 (06.01) Air-cooled xenon-arclamp operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Air dry coatings nonvolatile content oflatexes, test, 0 4758(06.02) Airless spray application Sa Spray--Applied coatings testing industrial water-reducible coatings, guide, 0 4712 $6.01) Air particulate filter samples lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (06.02) Alcohol-benzene-soluble content alcohol-benzene soluble matter in cellulose, test, D 1794 (06.02) Alcohol content; alcohol confent/purity of acetate esters, by gas chromatography, test, D 3545 (06,03) polyhydric alcohols in alkyd resins, qualitative analysis, test. D 2998 (06.02) Alcohol resistance wood furniture lacquers, test, 0 2571 (06.01) Alcohols (C4-C,3) plasticizer grade, chemical/pbysical analysis (selection/use of test procedures), E 852 (06.03) Aldehydes peroxides in styrene monomer, test, 0 2119 (06.03) purity of aldehydes and ketones, test, D 2192 (06.03) presence of and'removingmicrobial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) Aliphatic hydrocarbons ,J-nSee Hydrocarbons--aliphatic Alkaline cresylate solutions cresylic acid content (of alkaline cresylate solutions), chemical analysis, D 3439 (06.03) -- Alkaline earth carbonates----- - `` acid-insoluble extenders in (iron/copper phtlialocyanine/ ultramarine) blue pigments, test, D1135 (06.02) Alkalinity alkalinity in acetone, test, D1614 (06.03) Alkali resistance clear/pigmented organic coatings, test, 0 1308 (06.01) dried varnish films, test, D 1647 (06.01)' Alkyds/alkyd resins alkyd resins, selection of test methods, practice, 0 2689 (06.02) artists' paints (oii/resin-oil/alkyd), spec., 0 4302 (06.01) dichlorometliane/l,l,i-trichloroethane content in paints/ coatings, by direct ihjection gas chromatography, test, 0 4457(06.01) fatty acid content, test, 0 1398 (06.02) glycerol/ethylene glycol/pentaerythritol in aikyd resins, test, 01615 (06.02) identification of carboxylic acids in alkyd resins 0 2455 (06.02) identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, 0 2456 (06.02) 1135 DUP050298311 Alkyds/alkyd resins Index of ASTM Standards, Section 6 isophthalic acid content of alkyd/polyester resins, test, D 2690 (06.02) phthalic anhydride content (in absence of dibasic acids); test, 0563(06.02) phthalic anhydride content (in presence of dibasic acids), by gravimetric test, D 1306 (06.02) polyhydric alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) , rosin acids content, test, D1469 (06.02) specific gravity at 25/25C, test; 01963 (06.0 testing industrial water-reducible coatings, gmde'. D 4712 (06.01) unsaponifiable matter content, test, D 1397 (06X)2b <' All-day testing See Twent)'-tour hour testing 1 1 ; Alternative indicator method total, primary, secondary, and tertiary amine values.dffatty amines, test, D 2074 (06.03) Alumina ' acid-soluble extenders in (irdn/cdpper phthalocyanine/ ultramarine) blue pigments, test, D 1135 (06.02) 7 alumina/iron oxide in magnesium silicate pigment, test;D 717 (06.02) Alumina hydrate , '' i acid-insoluble extenders in (ircn/copper phthalocyanine/ ultramarine) blue pigments, test, D1X35 (06.02) Aluminum : '! acid/mortar resistance of factory-applied clear coatings oil'; ' extruded aluminum products, test, D 3260 (06.01) preparation of aluminum/aluminum4lteysatiKes'(for painting), practice, D1730 (06.01) preparation of hot-dip aluminum surfaces (for paintihg), practice, D1731 (06.01) Aluminum alloys 1* preparation of aluminum/aluminum-alloy surfaces (for painting), practice, D1730 (06.0I) , ' preparation of hot-dip aluminum surfaces (for painting), practice, D 1731 (06,01) Aluminum coatings See Coatings--aluminum , , Aluminum oxide (A12O>) content aluminum oxide in aluminum silicate (hydrous/anhydrous), , pigment, test, D 718 (06.02); aluminum oxide in titanium dioxide (Ti02)pigments, test, , D1394 (06.02) Aluminum potassium silicate - See Mica pigment Aluminum powder and paste Sa Pigments (headings) * ': aluminum powder/paste pigments for paints, spec., D 962 (06.02) sampling/testing flaked aluminum powders/pastes, methods, D 480 (06.03) Aluminum reduction method total titanium in white titanium pigments, by aluminum reduction method, , test, D1394 (06,02) Aluminum silicate pigments ,, aluminum silicate (hydrous/anhydrous) pigment, analysis, test, 1) 718 (06.02) aluminum silicate pigments (anhydrous), spec., D 361$ (06.02) aluminum Silicate pigments (hydrous), spec., D603 (06.02) American turpentine See Turpentine Amidoamines See Patty amidoamines Amine resins Sa Resins (.headings) amine resins--solvent tolerance, test, 01198 (06.02) ' Amines See Fatty amines Amines content Amine value acid/amine value of fatty quaternary ammonium, ehlsSll . D 2076 (06.03) , , TIS1 Amine values (total/primary/secondary/tertiary).riL*, fatty amines/amidoaminesAIiamines, hy refeiv oorenon method, test, D 2073 (06.03) fatty amines, by.alternative indicator method, test nSPi D2074(06.03) ' Aminolysis . identification of polyhydric alcoholsin alkyd resins, qualitative/quantitative analysis, test, D 2436 (06(02) Amino resins ', amino resins, selecting test procedures, practice, 1> 4277 ( free formaldehyde content of amino resins, test 0 197/ Ammonium hydroxide content ammonium hydroxide group {alumina/iron oxide) >n magnesium silicate pigment, test, D 717 (06 02)' 1 Amyl acetate primary (synthetic) amyl acetate (98 % grade), sxc D 3540 (06,03) ,, Amyl alcohol (synthetic) amyl alcohol (synthetic), spec., D 319 (06.03) Anatase-rutile ratio ratio of anatase to, rutile, in titanium dioxide (-Ii<>; pigment x-ray diffraction, test, D 3720 (06.02) *' , Angle of incidence * gloss differences between surfaces of similar app.urauurijie for visual evaluation, 0 4449 (06bl) * SB" Aniline industrial grade aniline, ?pep,, D 3264 (06.03) ( nitrobenzene aniline, test, 0 4589 (06.03) sampling and handling aniline, practice, D 3436 Aniline point ` aniline point/mixed aniline,point of petroleum products'v,'i hydrocarbon solvents, test, 0611 (06.03) sampling and testing dipentene, method, D 801 (06.03)Cj' Animat' black 1 See Bone black w ANSI replacement ,standards mUF use of protective coating standards in nuclear power planter selecting ATM standards, guide, 0 5144 (06,01) Anti-corrosion pigments--bask lead silicochromate., basic lead silicochromate pigment, spec., D1648 (06,02) chromium trioxideeohtent of basic lead sUicoschromaters pigment, test, 0 1844 (06.02) , Anti-corrosion pigments--red lead . jig rf lead peroxide/true red lead content of dry, red lead pi mcutS)'"' * test, D 49 (06.02) red lead pigment, spec., D 83 (06.02) Anti-corrosion pigments--strontium chromate chemical analysis of strontium chromate pigment, test, 01845 (06,02) . strontium chromate pigment, spec., D1649 (06.02) Anti-corrosion pigments--zinc chromate analysis, D 444 (06.02) zinc yellow (zinc chromate) pigments, spec., 0 478 (06.02) Anti-corrosion pigments.--zinc hydroxy phosphite analysis, 0 4450(06.02) zinc hydroxy phosphite pigment, spec., D 4462 (06.02) " Antifouling coating system erosion testing of antifouling paints, using high velocity water, . test, 0 4938(06.01) organotin release rates of antifouling coating systems in sea water, using graphite furnace atomic absorption spectrophotometry (GF-AAS), test, D 5108 (06.01) 1136 DUP050298312 Index of ASTM Standards, Section 6 Ash content--paints/related coatings/materials allow submergence test, D 3623 (06.01) Objecting marine antifouling coating to bifouiing and fluid shear forces in natural seawater, test, D 4930 (06.01) ouling paint pigments--copper powder irmical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) Jggpec powder (for antifouling paints), spec., D 964 (06.02) ng paint pigments--cuprous oxide %emical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) uprous oxide (for antifouling paints), spec., 0912 (06.02) 'ouling paint pigments--mercuric oxide Analysis, D 284 (06.02) mercuric oxide for use in antifouling paints, spec., D 911 (06.02) fimony content antimony content'(low concentrations) in solids of liquid , coatings/dried films, by atomic absorption spectroscopy, test, 03717 (06.01) imony oxide Sa Pigments (headings) antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3717 (06.01) ' antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (06.02) itl-sas meter sag resistance of paints, using a multinotch applicator, test, D 4400 (6.01) pparent acetyl content fapparent acetyl content of cellulose acetate proprionate/ butyrate, test, A D 817 (06,02) .pparent tack , , apparent tack of printing inks/vehicles, by inkometer, test, D4361 (06.01) ppearancc of materials bleeding characteristics, of dry pigments, test, D 279 (06.02) - blistering (of paints/related coatings), A D 714 (06.01) chalking (of white/lightly tinted exterior paint films), practice, . A D4214 (06.01) cheeking (of exterior paints), test, A D 660 (06.01) i clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) clear/pigmented organic coatings, test, D1308 (06.01) cracking (of exterior paints), test, A D 661 (06.01) degree of rusting on painted steel surfaces, method, A D 610 (06.01) erosion (of exterior paints), A D662 (06.01) evaluating degree of bleeding of traffic/pavement marking paint, test, A D 868 (06.01) flaking (of exterior paints), A D 772 (06.01) gas checking/draft test (of varnish films), D1643 (06.01) hiding power of paints, by reflectometty, test, A D 2805 (06.01) hiding power -relative dry hiding power (of paints/relatied coatings), test, D 344 (06.01) laboratory evaluation of degree of bleeding of traffic/pavement marking paint, test, D 969 (06.01) preparing drawdowns of artists' paste paints, practice, D 4941 (06.01) printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) selection/preparation of coating specimens, practice, D 3964 (06.01) testing industrial water-reducible coatings, guide, D4712 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, D 5146 (06.01) Application properties testing industrial water-reducible coatings, guide, D 4712 (06.01) Application viscosity (for paints/related products) high shear viscosity (of paints/vamishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Aqueous coatings sag resistance of paints, using a multinotch applicator, test, D4400 (06.01) Aqueous leachates (in pigments) water-soluble Salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) Aqueous slurries See Slurries Architectural coatings blocking resistance of trade sales paints, test, D 4946 (06.01) evaluating architectural paints for purchase by state/local governments, practice, D 3927 (06.01) index to selection and use of testing procedures, D 2833 (06.01) interior latex semigloss/gloss paints, selecting test methods, guide, D 4540 (06.01) leveling of aqueous/nonaqueous paints (in light/white tints), by draw-down method, test, D 4062 (06.01) practical washabiKty of organic coatings, test, D 4828 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, D 5146 (06.01) wet-to-dry hiding change of architectural coatings, test, D 5007 (06.01) Architectural paints and coatings hiding power of architectural paints applied by roller, test, D 5150 (06.01) print resistance of architectural paints, test, D 2064 (06.01) Architectural sandstone. preparatory surface cleaning of architectural sandstone, practice, D 5107 (06.01) Aromatic hydrocarbons See Hydrocarbons (headings) Aromatic potentiometer titrator acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D4370 (06.01) Aromatics content aromatics (ethylbenzene and eight-carbon (CB/heavier) content in mineral spirits, by gas chromatography, test, D 3257 (06.03) chemical analysis of benzene, by gas chromatography, test, D 4492 (06.03) Arsenic content arsenic in paint, test, D 2348 (06.01) Arsenic trisulfide See Qrpiment content Artists' paints --- 1 artists' acrylic emulsion paints, spec., D 5098 (06.01) artists' paints (oil/resin-oil/alkyd), spec., D4302 (06.01) artists' waitercolor paints, spec., D 5067 (06.01) labeling art materials for chronic health hazards, practice, D 4236 (06.01) lightfastness of pigments (in artists' paints), test, 0 4303 (06.01) preparing drawdowns of artists' paste paints, practice, D 4941 (06.01) ' relative tinting strength of chromatic paints, test, D 4838 (06.01) Asbestine See Magnesium silicate Ash content soluble cellulose nitrate, testing, methods, D 301 (06.02) Ash content--paints/related coatings/materials add/amine value of fatty quaternary ammonium chlorides, test, D 2077 (06.03) ashing cellulose, test, D 3516 (06.02) cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, D 871 (06.02) drying oils and fatty adds, test, D 1951 (06.03) 1137 DUP050298313 Index; of ASTM 'Standards, Section 6 Ash content--paints/related coatings/materials ethylcellulose, test, D 914 (06.02) , hydrogen .sulfide/sulfur dioxide (quaiijitative) of industrial aromatic hydrocarbons, test, D. 2363 (06.02) hydroxyethylcellulose, test, D 2364 (06.02) ' methvlceilulose, test. D1347 (06.02) moisture content of pigments, D 1208 (06.02) rosin, after burning and ignition, test.D 1063 (06.03) . sampling and testing pine tars/pine-tar oils, method, 0856(06.03) . sampling/testing lac resins (orange shallac/bgttbh 'lac/garnet lac/bleached lac), test,1 D 29 (06.02) ' tall oil, methods of testing, D 803 (06.03) Atmospheres---conditioning/testing standard environments for conditioning/testing paint/ , varpish/lacquer/reiated materials, spec., b'3924 (06it|l) Atmospheric analysis'' ^, desigri/fabricatibn of flue,gas des,uJfurizatiori system contponents (fop protective lining application), spec., (06.01) inspection of linings in operajting flue gas desulfurization systems, practice, D46i9 (06.01) Atomic absorption. See Spectrophotometry--atomic absorption Atomic absorption spectrophotometry See Spectrophotometry-rratomio absorption a, Atomic absorption spectroscopy ' See Spectroscopy---atomic absorption ?. Automatic spray ; - :` < producing films of uniform thickness of paint/varailsh/TdateEl i> products.on test panels, test, D 823 (06.01): > '" ns > 2I Automotive coatings/paints ' e amount of volatile organic compound (VOC) released from ' solventborne automotive coatings andiavdiiableibr > ' :* . removal 'in a VOC control device (abatement), test, i ' D 5087 (06.01) .i..,;; gloss of high-gloss metallic/nonmetallic surfaces, bygorriophotometry, method, E430(06.01) transfer efficiency under production conditions for spray.. application of automotive paints, by weightibgsis, practice, D5066 (06.01) , , viscosity of paints/reiated materials, by ISO flow cups, test,,,, .. D5125 (06.03) . V Bac-dray bleached lac ' See Bleached lac ' Backfill , . i ............ ' .impact resistance of pipeline Coatings, by limestone drop test,' G 13 (06.01) 'y - '' ' penetration resistance of pipeline coatings, bybiurif'rod test, G 17 (06.01) !; Bacteria/bacterial control ' '" resistance VS tnold growth on'surface Bf interior'paint (in an environmental chamber), test, D 3273 (06.01).' Bacteria/bacterial control--paints/related cogtirigs/maieriais resistance of emulsion, paints (in containers) tq attack by . microorganisms, test, D 2574 (06,01) . ' resistance to mold growth on surface of interior pain} coatings (in an environmental chamber); test, P 3273 (06.0i) Baked coatings nonvolatile content oflatexes, test, p 4758 (06.02) Baker-Philippoff equation ,. intrinsic viscosity of cellulose acetate, using modified Baker-PhiUppoff equation, test, D 871 (06.02) Baking (paints/reiated coatings) effects of overbaking on organic coatings, practice, D 2454(06.01) Balanced beam scrape adhesion and mar tester mar resistance of organic coatings,, using balanced beam scrape adhesion and mar test, D 5178 (06.01) .. Ball drop method . s , r visco0si1ty3,,4p3fc(0el6lu.0lo2s)e derivatives>* by baulkuirioopn v Barcodes f ,-sC abrasion resistance ofprinted^atter, t~. -in ,,., sive abrasion test, 13 5i8'l (06.01) ' 'I "`gj Barite See Barmin sulfate pigments ` .'is 1 f~ Barium sulfate r 1 " `fe'tfSgtB arid-soluble exfeniieiS Iff (irbd/cojipe- 'pinb.iluL .ji.i frJ&Ml Mtrajnarine) blue pigments, test, D j < >* (ifc42frV*`Hsi Barium sulfate content barium sulfate content in bariunPsUlfatemigmmf^rTM D 715 (06.02) - Sa Pigments (general properties) ,i_ barium sulfate pigment, analysis, test, Di|A lObDi)"1 Kf barium.SBlfate,.pigrrientSj spec,,;P602 (06,t)2) ij? Barriers - :.t> .< - 'xlajPjM comparative corrosion preventive charaefr si ,,.i n ttc\i used forjoints/couplings/fittings/patncsn u.n h ' cpatings, test, -G 18 (06.01) ' Bartlet whitelead; ,, ti ,See 'iBasic sulfate white lpad / , Barytes "` ,,, yWnJPft barium stdfa}eipig!neot^i4psc.,,p 602 (06.02) Base content icU. '* acid/base milliequivalent content ioi,f,fa>n*.o'sriir/ratrh. wM^tsl,Sg electroqqat bath^thqi^ ultraffijrates, test, 13 4W(l(r9 Basic carbonate'white lead - , .* J5- basic carbonate white lead pigment, spec., 13 61 (06!liS!r| white lead- chemical analysis, test, D1303 illii if* " . Basic lead silicochi'dhtitte \ 1 *''"5" baric lead silicochromate pignieut, sp6c., 11 lfe48'(O#'02fSS chromium trioxide content of basic lead sdico-chmMHr^ pigment; tesq D 1844 (06.02) 1 Basic sulfate white lead '> ,v ee3B white lead- chemical analysis, test, D 1303 (06 03} "jfc Beilsteihiinalysis . ,, , field identffication'orc0atings,itesti, 05043 (06 OTjbd|34 Bend testing--coatings. rv , effects of outdoor weathering on pipeline!! oati i s test, *.v G11 (0S.OI)! V x .. t .'Js m mandrel,betid test of'attached organic coat at s tcsrSS'MiSS _D5i2(Qfeai); ,I,-mmStS specific bendability of pipeline coatings, test <? 1(1106 Benzene : . ; ,v,,. acidity of benzene/toluene/xylenes/soivent n.iphtl as'si industrial aromatic hydrocarbons, tesi D 847 (Oft acid wash color, test1,.D848 (06.03),J .. .r. ,, apparent, density of industrial aromatic,hydioparbon^^M D 2935 (06.03) ^ aromatic hydrocarbons/related chemicqls,. terminolng>,'^,s, D47g0,(06.03) benzehe.qpntent in. hydrocarbon solvent,,by.gas c hroiuawKi raphy,. iest, D4367(06.03) " ! carbon ' AL`; *-" - Ch'criiical i ____ ________ , _____________ , D 4492 (06.03) " " f<*i commercial density (of purS liquid'chemicals), test' D 3505 (06.03) cyclic-hydrocarbcm products, by gas chroma! ign-ph \ tEssJ' D 4534 (06.03) 1> distillation, test^ D 850 (06.03) "1 ' impurities in high-purity ethylbenzene, by gas test,5060 (06.03)1 ...... ,.i . purity/benzene content of cyclohexane 995 l ,->l raphy, test, D 3054 (06.03) 1138 DUP050298314 Index of ASTM Standards, Section 6 Broad-band filter reflectometry ty of hydrocarbons from freezing points, test, I) 1016 (06.03) ned benzene-485 (nitration grade), spec,, 0835 (06.03) ned benzene-535, spee,, 0,2359 (06;03) ned benzene-545, spec., D 4734 (06.03) pling/handling liquid cyclic products (at ambient , , temperature), practice, 03437,(06.63) . 'dificatiou pqint, test,; D 852 (06.03), ophene content ofbenzene, by spectrophotometry, test, D 1685 (06.03) phene content pfrefmed-benzqhe, by. gas chromatography (with flame photqmetrie'.detectian), test, D 4735 (06.03) tal non-aromatic/trace monocyciic hydrocarbon arpmatic hydrocarbons,ip high-purity jpenzcne/toluene/jrmxed zylenes, by gas chroriiatograpliy,' test, 0 2360 (06.03) Olume/weight of industrial aromatic hydrocarbons, method, : D1555 (06.03) '' white See Basic carbonate white lead dal pigments \ See Antifouling paint pigments'(headings)t. ! tgrioratiqn ... ,,,, , See .beterioration . <...... , ,' ^ ogical data analysis Ejecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test,D4939(06,Olj Sfltpflng/'fiandling'4JL tsoMopylidene' fliphenol.{jpisphqqpl-A), J practice, 0 4297t06.tM) ' :' lidification point of 4,4- isopropylidenediphenol (Bisphcnoi A), test, 04493 (06.03). , . ; ' , lu'tiOn Color of 4;4'-isopf'Ppyiidetiediphbnol (dissolved in methanol), test, D 4789 (06.03) ' sninous materials (general) ' ` enetration resistance of pipeline coalings, by blunt rod test, G 17 (06.01) ;; listance of steel pipeline coatings to abrasion, by slurry of coarse.abrasive/wajer, test, G6 (06.01) ... tier in petroleum products/bituminous materials, by - distillation, test, 0 95 (06.01, 06.03) k box exposure test . ,> celerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (06.01) . , iron oxide . , Sees Iron oxide black, , pigments See Bone black pigment Set Carbon black pigment Lampblack pigment -, de applicator reducing fihna of uniform thickness of paint/varnish/rel,ated products on test panels, test, D 823 (06.01) . :c fixe < >. rSee Pigments (headings) ,: -clcanedsteel profile of abrasive blast-cleaned steel surfaces, in laboratory/ field/fabricating shop, test, 0 4417 (06.01) cleaning ndard pictorial surface preparation standards for painting steel surfaces, A D 2200 (06.01) bached lac pry, regular and refined, spec., 0 207 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, 0 29 (06.02) ding : . bleeding characteristics, of dry pigments, test, D 279 (06.02) evaluating degree of bleeding of traffic/pavement marking paint, test, AD868 (06.01) laboratory evaluation; of degree of bleeding of traffic/pavement s marking paint, test, D 969 (06.01) Blended silane-siloxane materials nonvolatile content in silanes/siloxanes/silane-siloxane blends used in masonry water-repellent treatments, test, D 5095 (06.01) Blistering evaluating degree of blistering, test, A 0 714 (06,01) testing water resistance of coatings, using controlled condensation, practice, 0 4585 (06.01) testing water resistance of coatings, using water fog apparatus, practice, 0 1735 (06.01) Blocking blocking resistance of trade sales paints, test, 0 4946 (06.01) organic coatings on wood substrates, test, 0 2793 (06.01) pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06.0]) Blotching reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) Blue-light reflectance ,. See . Reflectance and reflectivity (headings) Blue pigments Sa Iron blue/Phthalocyanine blue Ultramarine blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, D1135 (06.02) Blunt rod test penetration resistance of pipeline coatings, by blunt rod test, G 17 (06.01) Boiled oils (drying) See Oils (headings) Boiling point industrial aromatic hydrocarbons, test, 0 850 (06.03) Boiling water resistance wood furpiture Iqcquers^test, 0 2571 (06.01) Bonding , comparative corrosion preventive characteristics of materials, used for joints/couplings/fittings./patcbes in pipeline coatings, test, G18 (06.01) Bond strength bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) Bone black , -bpnqblackpigment, spec., 0 2l0 (06.02) solvent extractable material in black pigments, test, D 305 (06.02) Bone-dry bleached lac See Bleached lac--dry -- Book covers ____ abrasi0n, resistance of printed matter, by thega-eat comprehen sive abrasion test, 0 5181 (06.01) Boron trioxide (B?OJ calcium borosilicate, test, D 4487 (06.02) Brabender moisture tester moisture content of (iron/copper phthalocyanine/ultramarine) blue pigments, by Brabender test, 01135 (06.02) Break drying oils, test, D 1952 (06.03) Breaks cathodic disbonding of pipeline coatings, accelerated procedure, lest, G 8 (06.01) Brick bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06,01) Brightening power See Tinting strength Broad-band filter reflectometry directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) 1139 Mi DUP050298315 I ISfe&fwIlB-aa; Index of ASTM Standards, Section 6 Bromide content titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D 4764 (06.01) Bromine index aromatic hydrocarbons, by coulometric titration, test, D1492 (06.03) Bronze blue See Iron blue1 Bronze powders See Gold bronze powder Brookfield viscometer See Viscometers--Brookfield Brown iron oxide Sa Sienna (burnt and raw) Umber (burnt and raw) chemical analysis, method, D 50 (06.02) iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.62) synthetic brown iron oxide pigment, spec., D 3724 (06.02) Brunswick blue See Iron blue Brunswick green See Chrome green Brush-application behavior ' testing industrial water-reducible coatings, guide, D4712 (06.01) Brush drag comparison of the brush drag of latex paints, test, D 4958 (06.01) Brushes preparation of paint brushes for evaluation, practice, D 5068 (06.01) Bubble test viscosity of transparent liquids, by bubble time method, test, D 1545 (06.01, 06.02, 06.03) n-Butyl acetate alcohol content/purity of acetate esters, by gas test, D 3545 (06.03) 'H j*. n-buty! acetate (all grades), spec., D 4615 (06.03) , V' MT n-Butyl acrylate ... tffim n-butyl acrylate, spec,, B 3547 (06.03) -laMB purity, by gas chromdtography, test, D 3362 (06.03), .! unreacted monomer content of latexes using cap;]!a gas chromatography, test, D 4827 (061112) H' -Butyl acrylate/methacrylate unreacted monomer content of lhtexes, by chromatography, test, D 4747 (06.02) n.iii.-hcjincf. * k n-Butyl alcohol n-butyl alcohol (butanol), spec., D 304 (06.63) sec-Butyl alcohol' , " sec-butyl alcohol, spec,, D 1007 (06.03) " Butylated melamine-formaldehyde resins ' q) See Resins , , 'Ji Butylcatechol inhibitor content _ "J? p-tert-butylcatechol (TBC) in styrene monomer. iesE,<3g D 2120 (06.03) 'f residual p-len-butylcatechol (TBC) in styrene monSt?! additioh of NaOH, test, D 4590 (06.03) ' Butyl glycol * See Butoxyethanol 1 n-Butyl methacrylate unreacted monomer content of latexes using cap I gas Chromatography, test, D 4827 (06.1)21 _ 5 Butyraldehyde ' ,1 Sa Resins (headings) ,. poly(vinyl butyral)- chemical analysis, test, U139 Butyryl content ' cellulose acetate propionates, test, A D 8r Bulk density See Density--apparent (bulk) Burning characteristics--paints/related coatings/materials fire retardancy of paints, by cabinet method, test, A D1360 (06.01) small-scale evaluation of fire-retardant paints, by 2-foot tunnel method, test, D 3806 (06.01) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D 4206 (06.01, 06.03) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) Burnt sienna " Sa Pigments {headings) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, tesf, D.50 (06.02) raw/burnt sienna pigments, spec., D 765 (06.02) Butadiene purity of hydrocarbons from freezing points, test, D 1016 (06.03) Butane purity of hydrocarbons from freezing points, test, D 1016 (06.03) 1-Butanol See n-Butyl alcohol 2-Butanol See sec-Butyl alcohol 2-Butanone See Methyl ethyl ketone (MEK) Butoxyethanol 2-butoxyethanol, spec., D 330 (06.03) Button lac orange shellac and (button fac/garnet lac), spec., D 237 (06.02) sampling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, D 29 (06.02) C,-Cj3 alcohols chemical/physical analysis, selection/iise'bf ICSffirtj E 852 (06.03) Cabinet method fire retardancy of paints, by cabinet method, tesf? V AD 1360 (06.01) ' Cadmium content 1 "i lead/cadmium/cobalt content (low concentratiA0s|l nonvolatile portion of liquid coatings/dilud lifin atomic absorption spectroscopy, test, D 3335 (06.(il) Calcium borosilicate /'''Ji? analysis, D 4487 (06.02) S' calcium borosilicate pigments, spec., D 4288 Calcium carbonate calcium carbonate pigment, spec., D1199 (06 02)1 ,, Calcium content t calcium/zinc content, by EDTA method, lest, D 261 metals (iron/copper/manganese/calcium) contejit*Ji.' pulp (from wood/cotton), by atomic spectrophc test, D 4085(061)2) zinc dust (metallic zinc powder), test, D521((Jo.(12' Calcium oxide (CaO) content 1| calcium borosilicate, test, D 4487 (06.02) 1 calcium oxide in magnesium silicate pigment i-st, D 717 (06.02) Calcium paint driers See Driers -. Calculating test results ' calculating formulation physical constants of paintvcc practice, D 5201 (06.01) ' >' t 1 Calibration * conductivity cell for conductimetric analysis afwatsrs ionic contamination of blasting abrasives,1 test/- D 4940 (06.01) }T 1140 Con tent,: |4Tf Itedf.' id m feis KM parb{ astat' CcUif DUP050298316 Index of ASTM Standards, Section 6 ibration--paints/related coatings instrumentation uipment/standards for measuring purity ofpropylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) 'nreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) isity of printing inks/vehicles, by Ming-rod viscometer, test, D4040 (06.01) acitance mparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G 18 (06.01) illary gas chromatography analysis of styrene by capillary gas chromatography, test, D 5135 (06.03) tmreacted monomer-content of latexes using capillary column gas chromatography, test, D 4827 (06.02) pillary-moisture relations 'capillary moisture in concrete,-by plastic sheet method, test, D 4263 (06.01) rbou-arc lamps [accelerated testing of paints/varnishes/laequers/related products, using filtered open, flame carbon-arc light/water exposure w .apparatus, practice, D 822 (06.01) conducting tests on paint/varnish/lacquer/related products, - - using enclosed carbon-arc light/water.exposure apparatus, practice, D 5031 (06.01) operating carbon-arc light-exposure apparatus with and without u water for exposure of nonmetallic materials, practice,- G 23 (06.01) operating unfiltered apparatus (for testing paints/related coatings), using, the De.w cycle, practice, D 3361 (06.01) rbonate content acid-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D1135 (06.02) rbon black carbon black pigment for paint, spec., D 561 (06.02) solvent extractable material in black pigments, test, D 305 (06.02) rbon black content solvent extractable material in black pigments, test, D305 (06.02) arbon disulfide content [ carbon disulfide content of aromatic hydrobarbons, using spectrophotometry, <test, D 2324 (06.03) boxyl content carboxyl content of cellulose, tefct, D 1926 (06.02) ! rboxylic acid (identification of carboxylic acids in ^lkyd resins D 2455 (06.02) -boxylic acids content alkyd resins, test, D 2455 (06.02) astor oil .dehydrated castor oil, spec., D 961 (06.03) hydroxyl value of fatty oils/acids, test, D1957 (06.03) raw castor oil, spec., 0 969 (06.03) ,< spectrophotometric diene value of dehydrated castor oil/derivatives, test, D 1358 ,(06.03) ellular plastics See Urethanes (headings) ellulose and cellulose derivatives alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) ashing cellulose, test, D 3516 (06,02) carboxyl content of cellulose, test, 0 1926 (06.02) cellufose/ceflulose derivatives, terminology, D1695 (06.02) cellulose (chemically refined), composition by chromatographic analysis, method, D 1915 (06.02) chain length uniformity, by fractional precipitation of cellulose nitrate, test, D1716 (06.02) chlorine content, test, D 2641 (06.02) Chain length uniformity dichloromethane/I,1,1 -tricnloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(06.01) dichloromethane-soluble matter content of cellulose, test, 03971(06.02) ethoxyl substitution in cellulose ether products, by gas chromatography, test, 0 4794 (06.02) hydrogen sulfide/sulfur dioxide (qualitative) of industrial aromatic hydrocarbons, test, 0 2363 (06.02) hydroxyethylcellulose, test, 0 2364 (06.02) in cellulose ether products methoxyl and hydroxypropyl substitution, by Zeisel-gas chromatographic technique, test, D 3876 (06.02) intrinsic viscosity ofcellulose, test, 0 1795 (06.02) methylcellulose, testing, D1347 (06.02) moisture in cellulose, test, D 1348 (06.02) nitrogen content of soluble nitrocellulose, by ferrous sulfate procedure, test, D 4795 (06.02) pentosans content of cellulose, test, 0 1787 (06.02) silica content, test, D 2438 (06.92) ' . sodium glycolate content of sodium carboxymethylcellulose, test, 01439(06.02) solubility in sodium hydroxide, test, 0 1696 (06102) soluble nitrocellulose-base solutions, methods of testing, 0 365(06.02) .' sulfur content, by X-ray fluorescence, test, D 2929 (06.02) temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D1211 (06.01) volatile/nonvolatile content (of cellulosics/eroulsions/resin solutions/shellac/varnishes), selecting test procedures, practice, D 4209 (06.02) Cellulose and cellulose derivatives--cellulose acetate (CA) cellulose acetate, methods of testing, 0 871 (06.02) Cellulose and cellulose derivatives--cellulose nitrate (nitrocel lulose) cellulose liitrate in alkyd lacquers, quantitative determination by infrared spectrophotometry, test, D3133 (06.01) dilution ratio for solutions, test, 0 1720 (06.03) soluble cellulose nitrate, testing, methods,. 301 (06.02) Cellulose and cellulose derivatives--ethylcellulose (EC) ethylcellulose, methods of testing, D 914 (00.02) Cellulose and cellulose derivatives--pulp metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cqtton), by atomic spectrophotometry, test, 0 4085(06.02) Cellulosic plastics--cellulose acetate butyrate (CAB) cellulose acetate propionate/butyrate, methods of testing, A 0 817 (06.02) Cemeat ~ bond strength of thermoplastic-traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) Cementitious linings inspection of linings in operating flue gas desulfurization systems, practice, 0 4619 (06.01) Centrifuge (high-speed for vehicle separation) See Vehicle separation--solvent-type paints Ceramic whitewares directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) Cerium content cerium content (of paint driers), by EDTA method, test, 0 3970 (06.03) Cerium paint driers See Driers Certification form certification of coating conformance form, D 5063 (06.01) Chain length uniformity cellulose, by fractional precipitation of cellulose nitrate, test, D1716 (06.02) 1141 DU P05 02 98317 Chalk , Index of ASTM Standards, Section 6 " Chalk See Calcium carbonate Chalking white/lightly tinted exterior paint films, practice, A D 4214 (06.01) Change in color See Color (headings) Channel black See Carbon black (headings) Char index fire retardancy of paints, by cabinet method, test, A D 1360 (06.01) Checking exterior paints, test, A D 660 (06.01) Chemical analysis--paints/related coatings/materials calcium borosilicate, test, 0 4487 (96.02) C4-C|3 alcohols, chemical/physical analysis (selection/use of test procedures), E852 (06.03) chemical analysis ofyellow/orange/red/brown pigments containing iron/maganese, test, b 50 (06.02) ethyl methyl pefttanol content/pnrity value of 2-ethylhexanol, by gas chromatography, test, D 5008 (06.03) sampling industrial chemicals, practice, E 300 (06.03) white linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (06.01) white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) zinc hydroxy phosphite, test, fl 4450 (06.02) ' Chemical-resistantlinings inspection of linings in operating fltie gas desulfurization systems, practice, D4619 (06.01) Chemical-resistant matcrials/products clear/pigmented organic coatings, test, D 1308 (06.01) Chemicals aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) chemical resistance of pipeline coatings, test, G 20 (06.01) clarity/cleanness of (rtonpigmented) paint and ink liquid's, by visual'examination, test, D 2090 (06.02, 06.03) clear/pigmerited organic coatings, test, D 1308 (06.01) dipropylene glycol monomethyl ether, spec., D 4856 (06.03) propylene glycol monomethyl ether acetate, spec., D 4835 (06.03) propylene glycol monomethyl ether, spec., 0 4837 (06.03) China clay See Aluminum silicate (hydrous) Chinese blue jSee Iron blue Chinese red See Chrome orange Chinese white See Zinc oxide Chipping and chip resistance paints/related coatings, test, A D 3170 (06.01) traffic paint, A D 913 (06.01) Chloride content--paints/related coatings/materials ethylcellulose, test, D 914 (06.02) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, 0 2363 (06.02) methylceliulose, test, D1347 (06.02) sodium giycolate content of sodium carboxvmethylcellulose, test, D1439 (06.02) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) Chlorinated hydrocarbons dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D4457 (06.01) Chlorinated pheitol preservative content wood products, qualitative test for, D 2921 (06.01) Chlorine content cellulose, test, D 2641 (06.02) epoxy resins/compounds, test, D 4301106 (m hydrolyzable chlorine content of iiqmd , D1726 (06.02) ` total chlorine content of liquid epoxy ,, t M1,J " 1847 (06.02) : ~> H9 Chloroform-insolubles content chloroforminsolublematterinoiticiai.il lost Chromate coatings '' Sai-? Sa'ai formability/adhesion of zinc-rich primer'chunvate vomi'e coatings (on steel), test, n 4146 (06.01) ' relative tinting strength of chromatic paints , liihlitin Chromatidty ' See Color (headings) Chromatic pigments zinc yellow (zinc chromate) pigments, spec 0 47x'(twJ Chromatography--gas (detergents) ' :."V methoxyl/hydroxypropyl substitution I products), by Zeisel technique, test,; rt 3876q6 W2 Chromatography--gas (paints/related coating.) '-a identification of oils and oil acids in solvent-iedui <I>W? test D 2245 (06.03) identiftcatibn of polyhydric alcohols in alt'd icsm, qualitative/quantitative analysis, tesl 1) 2456 (OS' Chromatography--gas (paints/related coatings/innfenuN acrylate esters, purity, test, D 3362 (06.03) 1 alcohol content/purity of acetate esters, b\ .9 3 chfli'rraui test; 0 3545 (06.03) analysis of major organic impurities in pl.eiiu' i>rodueeH;J> cumene process, by gas chromatographs icsi-tf.a'(.q D496I (06.03) l analysis of major organic impurities in phenol piodtp cumene process, by gas chromatographv, test, 04961(06.03) analysis of purities/impurities of styrene, Ust, 0 3962f( analysis of p-xylene, method, D 3798 (06 03) v analysis of styrene by capillary gas chromatographs. 05135(06.03) aromatics (ethylbenzene and eight-carbon t. I49 9 ( WR* mineral spirits, test, 0 3257 (06.03) benzene content in hydrocarbon solvents bv B.. uiifun^o- raphy, test, D 4367 (06.03) benzene content of cyclic hydrocarbon products,, te/gtel chromatography, test, D4534 (06.03) \t4ye chemical analysis of benzene, by gas chrciiijic^rupfiv uaju, D 4492 (06.03) 'J * dichloromethane/l,l,lTtrichloroethane cor.icm 111 pinata/% coatings, by direct injection gas chrom.itorijphv, test'- 0 4457(06.01) ' ethoxy! stibstitntion in cellulose ether prod lets, b\ gas chromatography, test, 0 4794 (06,02) !' ethyl methyl pentanol content/purity value of 2-ethjitajkjjL by gas chromatography, test, 0 5008 (06.1x3) ? fatty add composition, by gas-liquid ehroii..uogi<nhv of in esters,-test, D1983 (06.03) *' identification of carboxylic acids in alkyd icoinx 0 2455.(09, identification of polyhydric alcohols in alkvd lcsins, qualitative/quantitative analysis, test, I) 2456 (06,021 impurities in high-purity ethylbenzene, b; gas chromatonra test, D 5060 (06.03) ` monopentaerythritol in commercial pentaerythritol, te$Wi8| D 2195 (06.03) *V phenol content (of tar acid mixtures), by hq' . r-om, raphy, test, 0 3626 (06.03) if H pinene composition (of wood/gum/sulfate tuipentmi'). tesu'j Jffit D 3009 (06.03) purity analysis of isopropylbenzene (cumene), test,... .... ..... D 3760 (06.03) t3@$fP purity/benzene content of cyclohexane 991 In ,,us LUoruat-oc--. raphy, test, O 3054 (06.03) ''' 11 jkh* 1142 DUP050298318 Index of ASTM Standards, Section 6 Coatings rity of methyl (amyl ketone/isoamyl ketone), test, D3893 (06.03) rity of methyl ethyl ketone, using gas chromatography, test, D 2804 (06.03) Urity of methyl isobutyl ketone, by gas chromatography, test, D 3329 (06.03) )rity of propylene glycol monotnethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether I' acetate, test, D 4773 (06.03) : putative identification of polymers in emulsion painfs, by infrared analysis/pyrolysis-gas liquid chromatography, a practice, D 3168 (06.01) sidual vinyl chloride monomer content of. poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) Ivent composition analysis (of solvent-type paints), direct-injection technique, practice, D 3271 (06.01) thiophene content of refined benzene, with flame photometric detection, test, D 4735 (06.03) : total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, test, D 2360 (06.03) {uniformity (of traffic paint vehicle solids), practice, D 2743X06.01) unreacted monomer content of latexes, test, D4747. (06.02) | unreacted monpmer, content of latexes using capillary column gas chromatography, test, D 4827 (06.02) unreacted toluene diisocyanate content of urethane prepqly- mcrs/coatings, test, D 3432 (06.02) if volatile resin acids in tall oil/gum/wood rosin, by gas chromatography, test, 1) 3008 (06.03) . water content of water-reducible paints, by direct injection into , gas chromatograph, test, D 3792 (06.01) r xylene isomer analysis, by gas chromatography, test, J D 2306 (06.03) xylene, purity of ort/io-xylene, test, D 3797 (06.03) hromatograiphy--gas (solvents) , benzene content in hydrocarbon solvents, by gas chromatog raphy, test, D 4367 (06.03) solvent composition analysis (of soivent-type paints), direct-injection technique, practice, D 3271 (06.01) hromatography-^-paper cellulose (chemically refined), compositibn by chromatographic analysis, method, D1915 (06.02) Chrome green Sa Pigments (general properties) chemical analysis of phthalocyanine blue/green pigments, test, D 3256 (06.02) chrome green pigment, spec., D 212 (06.02) - yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) /Chrome yellow and orange chrqme yeilow/orange pigment, spec., D 211 (06.02) ' yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Chromium content--paints/related coatings chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3718 (06.01) chromium content of strontium chromate pigment, by thiosulfate method, test, D1845 (06.02) lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (06.02) zinc yellow (zinc chromate yfellow) pigment, test, D 444 (06.02) Chromium oxide green chrome oxide green pigment, spec., D 263 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Chromium pigments See Chrome green/Chrome yellow and orange .Sa Chromium oxide green/Lead silicochromate Zinc chromate (yellow) Chromium trioxide content chromium trioxide content of basic lead silico-chromate pigment, test, D1844 (06.02) Chronic health hazards See Hazards--health CIE color system1 degree of rusting on painted steel surfaces, method, AD610 (06.01) Citron yellow See Strontium chromate Clarity/cleanness clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D2090 (06.02,06.03) Classification field identification of coatings, test, D 5043 (06.01) Clay (aluminum silicate) See Aluminum silicate pigments Cleaning practical washability of organic coatings, test, D 4828 (06.01) Cleaning--drycleaning materials/tests mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) Cleaning solvents See Solvents Closed-cup flash point methods See Flash point (headings) Cloud point aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) Coalescence latex paint films at low temperatures, test, D 3793 (06.01) Coarse particle analysis Sa Dispersion Particle size (analysis/distribution).(headings) coarse particles in pigments/pastes/paints, test, D 185 (06.01, 06.02) reporting particle size characteristics of pigments, practice, D1366 (06.02) Coated pipelines See Pipeline coatings Coated substrate standards film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Coating adhesion adhesion ofcoating films to metallic substrates, by tape test, D 3359 (06.01) organic coatings, applied to smooth panel surfaces, by scrape adhesion test, D 2197 (06.01) Coating capacitance water penetration into pipeline coatings, test, G 9 (06.01) Coating contractors See Nuclear reactor vessels--qualifications for painters Coating industry design/use of safety alert system for hazardous work locations in . coating/lining industry, practice, A D4257 (06.01) Coating leveling See Leveling characteristics Coatings accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (06.01) accelerated testing of paints/vamishes/lacquers/related products, using filtered open flame Carbon-arc light/water exposure apparatus, practice, D822 (06.01) antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D3717 (06.01) 1143 DUP050298319 Index of ASTM Standards, Section 6 Coatings assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) certification of coating conformance form, D 5063 (06.01) chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3718 (06.01) clarity/cleanness of (nonpigmented),paint and ink liquids, by visual examination, test, D 2090 (06.02, 06,03) commercial hexanes, spec., D1836 (06.03) conducting a patch test to assess coating compatibility, practice, D 5064 (06.01) dichloromethane/l,t,l-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457(06.01) dry film thickness, by microscopical measurement, D 2691 (06.01) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) ` evaluating degree of settling (pigment suspervsion/ease of remixing a shelf-aged sample) of paint, test, D 869 (06.01) evaluating (interior/exterior) coatings for protecting steel Surfaces at high-temperature service, test, A D 2485 (06.01) d evaluation of (clear/pigmented) coatings for rigid/semirigid plastics substrates, practice, D 3002 (06.01) exposure of paints/related coatings to fluorescent UV- condensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) field identification of coatings, test, D 5043, (06.01) fineness of dispersion of pigment-vehicle systems, test, , 01210(06.01) lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/driedi films, by atomic absorption spectroscopy, test, D 3335 (06.01) ,, mercury content (low concentrations) in liquid coatings/coatings vehicies/dried films, by atomic absorption spectroscopy, test, 03624(06.01) photographic documentation of coatings/lining defects/failures, D 4121 (06.01) porosity of paint films (to indicate coating penetration), test, 03258(06.01) presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D4610 (06.01) producing films of uniform thickness of paint/vamish/related products on test panels, test, D823 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) ' purity of methyl isobutyi ketone, by gas chromatography, test, D 3911 (06.01) "sag resistance of paints, using a multinotch applicator, test, D 4400 (06.01) static friction of coating surfaces; test, D 4518 (06.01) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, 05146(06.01) testing water resistance of coatings at [00 % relative humidity, practice, D 2247 (06.01) . volume nonvolatile matter in clear/pigmented coatings, test, D 2697 (06.01) wood used as panels in weathering tests of coatings, spec., 0 358(06.01) Coatings--chromate formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, 04146 (06.01) relative tinting strength ofchromatic paints, test,- D 4838 (06.01) Coatings--coating work in nuclear facilities Sa Nuclear reactor vessels--qualifications for painters use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) Coatings--coil application using a wire-wound drawdown bar, practice 04147(06.01) coil coatings, testing, practice, D3794 (06.01) Coatings--enamel amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus practice, D 5031 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, by goniophotometry, method, E-430 (06.01) Coatings--epoxy subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater^ test, 1) 4939 (06.01) Coatings--organic - See Organic coatings. , Coatings--ultraviolet-cured cure time, practice, D 3732 (06.01) estimating package stability of coatings for ultraviolet Curing, test, D 4144(06.01) Coatings mbnitoring'program establishing procedures to monitor performance of safety related coatings in operatinghuclear power plant, guide, D 5163 (06.01) Coating thickness 1 disbonding characteristics of pipeline coatings, by direct soil burial, test. G19 (06.01) dry film thickness ofprotective coating systems, by destructive means, test, 1)4138 (06.01) film thickness ofpipeline coatings on steel, nondestructive measurement!-method, G 12 ;(06.Q1) Cobalt content .: lead/cadmiufo/cobaU content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D3335 (06.01) paint driers, by EDTA method, test, D 2373 (06.03) Cobalt paint driers Sa Driers liquid paint driers, selection of test methods, D 564 (06.03) Coconut oil coconut oil, spec., D1841 (06.03) Coefficient of friction static friction of coating surfaces, test, D 4518 (06.01)- Coefficient of retroreflection (of retroreflectors) See Retroreflection/retroreflectors Coffee stains wood furniture lacquers, test, D 2571 (06.01) Cohesive strength bond strength of thermoplastic traffic marking materials, using cemfeht bricks/steel cubes, test, D 4796 (06.01) Coil coatings application using a wire-wound drawdown bar, practice, D 4147 (66.01) coil coatings, testing, practice, D 3794 (06.01) Cold-check resistance temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D 1211 (06.01) Cold resistance temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D .1211 (06.01) Colloidal black See Carbon black (headings) Cologne yellow See Chrome yellow Color cellulose acetate propionates/butyrate, test, A T> 817 (06.02) 1144 DUP050298320 Index of ASTM Standards, Section 6 or--discoloration falear coatings, by sunlight-through-glass test, D 2620 (06.01) Jtear/pigmented organic coatings, test, D1308 (06.01) Stirfaces of paints/related coatings (by microbiological attack), practice for determining by exterior exposure tests, By D 3456 (06,01) ilor--light exposure |pferating carbon-arc light-exposure apparatus with and .without water for exposure of nonmetallic materials, practice, G 23 (06.01) Pf--lightfastness |htfastness of pigments (in artists' paints), test, D 4303 (06.01) tinted matter, D3424 (06.01) -organic/inorganic chemicals cetaldehyde, spec., D 4710 (06.03) pellulose acetate propionates/butyrate, test, A D,817 (06.02) Rotor of cresylic acids ("C1' series standafo(j5),,tesi, D 3627 (06413) atty acids (after heating), test,'!) 1981 (06.03) iiaieic/phthalic anhydride (in molten state/after heating), by platinum-cobalt scale, test, D 3366 (06.03) . nethyi acrylate, spec., 0'4709 (06.03) jjsampling and testing dipentene, method, D 801 {06.03) |lor--paints/related coatings/materials Buminum silicate (hydrous/anhydrous) pigment, analysis, test, D 718 (06.02) jjgrtists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) enzene/tbluene/xylenes/refmed solvent naphthas/simjlar industrial aromatic hydrocarbons, test, D84s (06.03). icellulose acet&te, test, 0 871 (064)3) polarity/cleanness of (honpigmehted) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06103) Jtelear liquids, by platinum-cobalt scale, test, I D1209 (06.01, 06.03) jgfsolor differences from instrumentally measured color differences of opaque materials, test, D 2244 (06.01) oldred pigtriente (dry/pastes in oil), with'a mechanical rhulier, p, test, D 387 (06.02) i color of transparent liquids, by Gardner color scale, test, 0 1544 (06:01, 06.02, 06.03) Icolor pigments, by miniature sandmill method, test, AD 3022 (06.02) Ijdrying oils (after heating), test, D1967 (06.03) Revaluation of color for thermoplastic traffic marking materials, test, D 4960 (06.01) ftmagnesium silicate pigment, analysis, test, D 717.(064)2) |preparation of standard color solutions (caramel/platinum- cobalt), for color test on soluble nitrocellulose-base solutions, D 365 (06.02) i quantifying dirt collection on coated exterior panels, test, D 3719 (06.01) ., J-heflection haze (of high gloss Surfaces), test, 0 4039 (06,01) H relative tinting Strength of chromatic paints, test, D 4838 (06.01) j sampling and testing pine tars/pine-tar oils, method, D 856 (06.03) sampling and testing turpentine, method, D 233 (06.03) sampling/testing lac resins (Orange shellac/button lac/garhet lac/bleached lac), test, D 29 (06.02) H solid aromatic hydrocarbons/related materials (in molten state), by platinum-cobalt scale, test, D1686 (06.03) ! solution color of 4,4'-isopropylidenediphenol (dissolved in methanol), test, D 4789 (06.03) testing industrial water-reducible coatings, guide,. D 4712 (06.01) lolorfastness lightfastness of printed matter, D 3424 (06.01) Olorimeter ! relative tinting strength of printing ink dispersions, test, D 2066 (06.01) blor index |P artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) Conformance Colorless monomeric acrylate esters methyl ether of hydroquinone (MEHQ) content of colorless monomeric acrylate esters, test, D 3125 (06.03) Comb gages wet film thickness of organic coatings, by notched gages, practice, D 4414 (06.01) Commercial cyclohexane See Cyclohexane 995 Commercial density See Density (headings) Commercial hexanes commercial hexanes, spec., D1836 (06.03) Comparison techniques evaluating and comparing transfer conditions-laboratory conditions, test, D 5009 (06.01) Compatibility.. conducting a patch test to assess coating compatibility, practice, D 5064 (06.01) factory-primed wood products with finish coatings, test, D 2830 (06.01) Composites--wood edge performance of composite wood products under surfactant accelerated moisturestress, test, 0 2065 (06.01) Composition analysis--paints/related coatings/materials chemical analysis of yfcllow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) Compressed air oil/water presence in compressed air (used for coating application/air blast cleaning/abrasive blast cleaning), D 4285 (06.01) Concentration (of elements) concentration of formaldehyde solutions, test, D 2194 (06.03) Concrete--paint applications sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Concrete--surfaces abrading concrete, practice, D 4259 (06.01) acid etching concrete, practice, D 4260 (06.01) capillary moisture, by plastic sheet method, test, D 4263 (06.01) continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) making and preparing concrete/masonrv panels for testing paint finishes, method, D1734 (06.01) pH of chemically cleaned/etched concrete surfaces, D 4262 (06.01) surface cleaning concrete (for coating), practice, D 4258 (06.01) surface Cleaning concrete unit masonry (for coating), practice, D 4261 (06.01) Condensation water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) Conditioning standard environments for conditioning/testing paint/ varnish/lacquer/related materials, spec., D 3924 (06.01) Conductance and conductivity (electrical) cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) electrical conductivity of electrocoat baths, test, D 4399 (06.01) Conductivity bridge/ceil electrical conductivity of electrocoat baths, test, D4399 (06.01) Cone-and-plate viscometers Sa Viscometers (headings) high shear viscosity (of paints/vamishes/related products), by IC1 cone/plate viscometer, test, D4287 (06.01) Conformance certification of coating conformance form, D 5063 (06.01) 1145 KM DUP050298321 ZZ86Z090dn d 9NI ' (10*90) 81 O `15SJ 5`s 8 < > ' 6o " oipdiJ ni saqoiEd/sSunHj/sSaqdnoa/siuiof > 7> pasn ' i%jtepsipp8mp 3AlJU3A3J(i UOISOJJOO aAIJEJEClUIOO |jj'|,;Y' , sanqdiKo (Z0'90) SIT O tsai 'sjoatuSid anjq (auuBiHB.uin/auiuEXooiBqiqd jaddoo/uoni) jo ^<^X> ' _' jEOioiaqo aiqq aiuuBXaoiBqjqj ng aniq auiireXooiBqiqd jaddo3 ,'i((T9&) I96 Q *IS3I `XiJ3uiO[noooiDim aAippixo unqiEooJpXq 8< < ' < 98> 'pmbi[ U[ (saiiiurenb :;' < <) jnjpis Xjpaiopoaojanu--Xjpiuo[no;j 11 It`t#) 196 a 'isai ',tii3uio[noooj3iui aAippixo ^'`suotpfiojp'ii iqEHioiEjpmbii ui (sapijirenb aaEjj) jnjpis * XflEiuo|no3 `d (0r90) Z6PIQ Ipskiuaiuoa aaimojq <> > `suoqjBaojpXq aijEtuojB W-' =>< > ' > > < >aujaiuiqno;) rnr ` (0*90) P8I a `M3ds '[10 paasuonoo H4' suoijBoypads--sppeX)jB,f gg Hl|kJ go paasnojpo ~Jk! 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sjured ajqpnpaj inaAios jo (|| ) spunodiuoa }< ~' S> 3[< < '[ JOSOJ3B--SjaUIBJU03 (10*90) Z9SG `isai bawinoasu latioois 3uisn`sjured jo Xauajstsuoo Xanaisisuoo (10*90) 1915 a `spins `sapuisqns |Bjatu no ijiOKv Siituii/SuijEoa > ]> sjuaiuajinbaj uoiioadsuiSuiXjpads 3JU[< ' > sSupBoa jo aauanbasao3 (sSmpvdxf) s[fo 33S sjio pajBSnfuo^ (0*90) 85I a `isai "saAiiBAuap/ito > > ' pajBjpXqap jo anjBA auaip ouiauuojoqdojpads auaip pa)B3nlbo9 (10*90) ZZS a `jsaj `sSnpBoa < ' S> paqoBUE jo isai puaq pjpuEui sujBjBddB (ajpuBui |Baiuo3 SPJBJBddB pjpUBlH JB31U03 it''' HBR: 9 uorpajs `spiBpuBJS HXSV jo xapuj Index of ASHi Standards, Section 6 Degradation- -paints/related coatings/materials coatings . continuity verification of liquid/sheet linings applied to concrete j, substfiltes, practice, D4787 (06.01) |dge performance of composite .wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) effects of outdoor weathering on pipeline coatings, test, G11 (06.01) . exterior paints, evaluating, test, A D 661 (06.01) mandrel bend test of attached organic coatings, test, | D 522 (06.01) Ipecific bendability of pipeline coatings, test, G 10 (06.Q1,). fesol . - . fmter content, by iodine reagent method, test, D1631 (06.03) gsylicacid. ,, \ s .. .ji.-sif-> . , and phenol, sampling and handling, practice, D 3852 (96,03) color of cmsylic acids ("C" .series standards), test, D 3627 (06.03) jpresylic acid content (of alkaline cresylate solution?), chemical analysis, D 3439 (06.03) , pyridine base content in cresylic acid,, by direct titration, test, 5 D 4471 (06.03) .- . oss-cut tape ..test adhesion ofcoating films to metallic substrates, by tape test, D 3359 <06.01) >oss-hatch tape test T- . adhesion of coating films to metallic substrates, by-tape test, D 3359 (06.01) ossindex (index of ASTM methods equivalent/rdated to methods in Federal Standard 141 ("Paint, Varnish, Lacquer, and Related Materials; Methods for Sampling and Testing"), (Related Material) (06.01, 06.02, 06.03) ide tar acids |i See Tar acids--crude/refined , stallization : solidification point of 4,4- isopropylidepedjphenol (Bisphenpl A), test, D 4493 (06.03) ; . :! T) specimen testing adhesion of coating films to metallic substrates, by tape: test, D 3359 (06.01) imene (isopropylbenzene) See Isopropylbenzene (cumene) mene process analysis of major organic, impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (06.03) f ( prous oxide chemicahanaiysis of cuprous oxide/copper pigments, test, D 283 (06.02) cuprous`oxide (for antifouliag paints); spee., D 912 (06.02) . ' ring characteristics : MEK resistance of ethyl silicate (inorganic) zinc-rich,primers, by solvent rub, test, D 4752 (06.01) ring of organic coatings See Drying or curing ring time stroke cure time of thermosetting phenol-formaldehyde resins, test, D 4640 (06.02) rrent measurement comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) nrtain coat : testing industrial water-reducible coatings, guide, D 4712 (06.01) t tape test adhesion of coating films to metallic substrates, by tape test, 0 3359(06.01) Cyanoacrylate adhesive adhesion of organic coatings to plastic substrates, by direct tensile testing, D 5179 (06.01) Cyclohexane apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) benzene content ofcyclic hydrocarbon products, by gas chromatography, test, D 4534 (06:03) commercial density (of pure liquid chemicals), test, D 3505 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D3437 (06.03) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) volume/weiOJit 6findustrial aromatic hydrocarbons, method, D1555 (06.03) Cyclohexane 995 cyclohexane 995, spec.; D 3055 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, D 3054 (06.03) Cylindrical mandrel apparatus mandrel bend test of attached organic coatings, test, D 522 (06.01) Damping hardness test hardness of organic coatings, i>y ly&nig/Persoz pendulum hardness iSsts, D4366 (06.01) ' Dark chrome yellow See Chrome yellow and orange Data analysis--recording/reporting results recording results on singie-/multi-panel forms, method, AD 1150 (06.01) Daylight Sa Reflectance arid reflectivity (headings) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E97 (06.01) Decomposition points industrial-aromatic hydrocarbons, in distillation tests, D 850 (06.03) Decontamination decontaminability of coatings used in light-water nuclear power plants, test, D 4256 (06.01) use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) Defects--coatings photographic documentation of.cpatrags/fining defects and failures, D 4121 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) Definition of terms naval stores/related products, def. of terms, D 804 (06.03) protective coating/lining work for power generation facilities, terminology, D4538 (06.01) Deformation--paints/related coatings/materials flexibility/adhesion oforganic coatings (paints) on prepainted deformed metallic sheets, test, D 4145 (06.01) formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (06.01) mar resistance of organic coatings, using balanced beam scrape adhesion and mar test, D 5178 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G 17 (06.01) resistance of organic coatings to effects of rapid deformation (impact), test, D 2794 (06.01) Degradation--paints/related coatings/materials accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D4141 (06.01) 1147 iMi |r 1*1 DUP050298323 Index of ASTM Standards, Section 6 Degradation--paints/related eoatings/materials conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D S031 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) water resistance of coatings, using controlled condensation, practice, D 4585 (06,01) Degree of cure See Curing characteristics Degree of dispersion See Dispersion Degree of settling evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, D 869 (06.01) Degrees of freedom aromatic hydrocarbons/related chemicals, terminology, 0 4790(06.03} Degummed soybean oil See Soybean oil Dehydrated castor oil See Castor oil Densitometer relative tinting strength of printing ink dispersions, test, D 2066 (06.01) Density--paints/related coatings/materials apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) calculating formulation-physical constants of paints/coatings, practice, D5201 (06.01) commercial density (of pure liquid chemicals), test, D 3505 (06.03) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxyethylceilulose, test, D 2364 (06.02) methylcellulose, test, D1347 (06.02) paint/varnish/lacquer/related products, test, A D 1475 (06.01) sodium glycolate content of sodium carboxymethylcellulose, test, D1439 (06.02) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Density--petroleum products volume/weight of industrial aromatic hydrocarbons, method, 01555(06.03) Dental tin foil substrate preparation of free films of organic coatings, practice, D 4708 (06.01) ' Deposition deposition efficiency of polymeric powders/powder coatings, practice, D 3451 (06.01) Depth of color See Color (headings) Depth of penetration penetration resistance of pipeline coatings, by blunt rod test, G 17 (06.01) Design--building applications design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) Design basis accident (DBA) use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.0.1) Destructively-distilled wood turpentine See Turpentine Destructive testing--coatings dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) Desulfurization systems design/fabrication of fluegas desulfm iz-uon s'i (for protective lining application), spc. I! ... ,, inspection of linings in operating fluegas diAuIf.iriAl systems, practice, D4619 (06.01) / Detergent materials/systems--drycleaning mineral (petroleum) spirits hydrocarbon dil spec., D 235 (06.03) " Detergent resistance ,* organic finishes, practice, D 2248 (06.01) 1V Deterioration water penetration into pipeline coatings, test, G 9 (tig o' Deterioration--biodeterioration ' J microbiological discoloration (of paint film surf, exposure tests, practice, D'3456 (06 01) paint films, evaluating degree of surface:disfigurement AD 3274(061)1) " resistance of eiiuilsion paints (in containers) to aide1 microorganisms, test, D 2574 (06.0]) resistance to mold growth on surface of iff erioi p'a{r,,, (in an environmental chamber), test D3273 (1)6 Dew cycle operating' ligLt- and water-exposure apparatus carbon-arc type), in testing paints and practice, D 3361 (06.01) ." Diacetone alcohol rtj| diacetone alcohol, spec., D 2627 (06.03) Diamines ' % Sjg See Fatty diamines Diatomaceous silica pigment JBSa Silica (diatomaceous) gldiatomaceous silica pigment, analysis, test I)' id ill 02 Dibasic acids (absence or presence) See Phthalic anhydride' content Dibenzal method monopentaerythritol iit commercial pentuciyliirnoi D 2195 (06.03) Dibutyl phthalate dibutyl phthalate, spec., D 608 (06.03) JBMl Dichloromethane * SI dichloromethane/1,1,1 -trichloroethane content in pain coatings, by direct injection gas chrematoerapn-,, D 4457 (06.01) '` dichloromethane-soluble matter content o.'cclluose, unit/ D3971 (06.02) 1**981 Dielectric constant (permittivity)/dissipation factor ., comparative corrosian preventive characteristics oi.ma' used for joints/couplings/fittings/patdics m pipeli coatings, test, G18 (06.01) A water penetration into pipeline coatings, test, G 0 (06.0 Diethylbenzene isomers impurities in high-purity ethylbenzene! by gas chromat^ test,' D 5060 (06.03) - yJjm Diethyleneglycol >i(^ I-' diethylene glycol, spec., D 2694 (06.03) flash/fire point ofliquids, by Tag open-cup apparatus, les^,/ D1310 (06.03) Difatty secondary amines See Fatty amines r Differences in color See Color (headings) Diffraction intensity (of x-rays) See X-ray diffraction Dillon dynamometer bond strength of thermoplastic traffic marking mats ta'si cement bricks/steel cubes, test, D 4796 (06.01)- Diluents paint/related coatings- odor (characteristic/residual},.test, D 1296 (06.03) tj 1148 DU P050298324 Index of ASTM Standards, Section 6 Driers 'lutabillty value |iesin solution diluiiabiUty, test, D 5062 (06.03) ution ratio/value cellulose nitrate solutions, for active solvents, hydrocarbon diluents, and cellulose nitrates, test, D 1720 (06.03) soluble cellulose nitrate, testing, methods, D 301 (06.02) mer, acrylic add dimer in acrylic add/unsaturated organic adds, test, D 4415 (06.03) methyl-benzyl alcohol , analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (06.03) {methyl ketone See Acetone ip application " testing industrial water-reducible coatings, guide, D 4712 (06.01) ip eoafer f producing films of uniform thickness of paint/varnish/relaled products on test panels, test, D 823 (06.01) - jpentcnc (and related terpene solvents) >" sampling atjd testing dipentene, method, D 801 (06,03) ipropylenc glycol dipropylene glycol, spec., D 2696 (06.03) ' i ' , propylene glycoi/dipropylene glycoH'spec., D 5164 (06.03) ipropylene glycol nionomethyl ether (DPM) dipropylene glycol monomethyl ether, spec., D 4836 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/ptopylene: glycol monomethyl, ether acetate, test, D4773 (06.03) jOip-type viscosity test ' viscosity (of pamts/vamishes/lacquers/related materials), by dip-type viscosity cups, test, D 4212 (06.01) Direct aspiration spectrophotometric procedure Sa Spectrophotometry (headings) lead content in paint, by direct aspiration atomioabsorption spectroscopy, test, D 4834 (06.01) Directionality ` gloss of high-gloss metaliic/nonmetaliic surfaces, by goniophoto- metiy. method, E 430 (06.01) Directionality of surface gloss differences between surfhees of similar appearance, method for visual evaluation, D 4449 (06.01) Directional reflectance 1 See Reflectance and reflectivity (headings) Dirt accubiulation Sa Soil accumulation . ' quantifying dirt collection on coated exterior panels; test, J D3719 (06.01) l! Dirt resistance See Resistance--soil Disbonding disbonding characteristics of pipeline*coatings, By direct soil burial, test, G19 (06.01) . specific bendability of,pipeline coatings, test, G 10 (06.01) Disbonding--cathodic cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) pipeline coatings subjected to high or cyclic temperatures, test, , G 42 (06.01) Discoloration See Color--discoloration Discontinuities--Coatings continuity verification of liquid/sheet linings applied td concrete substrates, practice, D 4787 (06.01) discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) Dispersion coarse particles in pigmentS/pastes/paints, test. D185 (06.01, 06.02) coppbr phthalocyanine blue pigment, spec., D 963 (06.02) fineness of grind of printing inks, by NHRI grindorneter, test, D1316 (06,01) Distillation--bituminous materials water in petroleum products/bituminous materials, by distillation, test, D 95 (06.01, 06.03) Distillation--paints/related coatings/materials cresyhc acid content (of alkaline cresylate solutions), chemical analysis, D 3439 (06.03) distillation of industrial aromatic hydrocarbons/related materials, test, D 850 (06.03) distillation of petroleum products, method, D 86 (06.03) distillation range (between 30 and 350C) of volatile organic liquids, test, D1078 (0603) ethyl acetate (all grades), spec., D 4614 (06.03) pine tars and pine tar oils, test, D 856 (06.03) sampling and testing dipentene, method, D 801 (06.03) sampling and testing pine oil, method, D 802 (06.03) sampling and testing turpentine, method, D 233 (06.03) vacuum distillation (for vehicle ,separation in solvent-type paints), practice, D 3272 (06;0l) Distillation--petroleum products, distillation of petroleum products, method, D 86 (06.03) water in petroleum products/bituminous materials, by distillation, test, D 95 (06.01, 06.03) Distilled fittty acids See Fatty acids--specifications Distilled water aridity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06,03) Doctor test mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) Dolomite See Calcium carbonate Double rub method MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) Douglas fir wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Draft test varnish films, test, D1643 (06.01) Drag comparison of the brush drag of latex paints, test, D 4958 (06.01) Drawdowns preparing drawdowns of artists' paste paints, practice, D 4941 (06.01) Draw-down test 1-- coil coatings, application using a wire-wound drawdown bar, practice, D4147 (06.01) leveling characteristics of architectural paints/coatings (aqueous/nonaqueous), in wbite/iight tints, D 4062 (06.01) paint spatter resistance to roller application, test, D 4707 (06.01) sag resistance of paints, using a multinotch applicator, test, D 4400 (06.01) Driers calcium/zinc content, by EDTA method, test, D 2613 (06.03) cerium content, by EDTA method, test, D 3970 (06.03) clarity/cleanness of (nonpigniented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) ' cobalt content, by EDTA method; test, D 2373 (06.03) iron in liquid iron paint driers, by EDTA method, test, D3804 (06.03) lead content, by EDTA method, test, D 2374 (06.03) liquid paint driers, selection of test methods, D 564 (06.03) liquid paint driers, spec., I>600 (06.03) manganese content, by EDTA method, test, D 2375 (06.03) rare earths content, by EDTA method, test, D 3989 (06.03) 1149 DU P050298325 G ' t'vSi.'fTr Driers Index of ASTM Standards, Section 6 .if , V *>* vanadium content, by EDTA method, test, D 3988-(06.03) volatile/nonvolatile content (of driers/drying oils/naval stores and solvents), selecting test procedures, guide, D 4140 (06.03) zirconium content, by EDTA method, test, D 3969 (06.03) Drop black See Bone black Drop tests impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) Dry bleached lac See Bleached lac Dry film thickness See Film--dry film thickness Drying oils See Oils--drying Drying or curing coatings, by ultra-violet techniques, practice for reporting cure time, D 3732 (06.01) MEK. resistance of ethyl silicate (inorganic) zinc-rich primers. By solvent rub, test, D 4752 (06.01) organic coatings, at room temperature, determination of film formation rates, test, D1640 (06.01) sampling and testing shellac varnish, D1650 (06.02) soluble cellulose nitrate, testing, methods, D 301 (06.02) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D3259 (06.01) Drying time sampling and testing shellac varnish, D 1650 (06.02) Dry red lead See Red lead Durability accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D 4141 (06.01) comparison of the brush drag of latex paints, test, , D 4958 (06.01); exterior durability (of varnishes), test, D1641 (06.01) factory-primed wood products with finish coatings, test, D 2830 (06.01) Dutch white See Basic carbonate white lead Dynamic viscosity See Viscosity (headings) Dynamometer testing bond strength of thermoplastic traffic marking materials, using cement bricks/steei cubes, test, D 4796 (06.01) Earth pigments See Ochre So Sienna (burnt and raw) Umber (burnt and raw) Ease of brushing comparison of the brush drag of latex paints, test, D 4958 (06.01) Eccentric center wheel wet film thickness gage wet film thickness of organic coatings, D 1212 (06.01) Eddy current examination See Electromagnetic (eddy current) testing Edge performance edge performance of composite wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) EDTA method calcium content in paint driers, test, D2613 (06.03) cobalt content in paint driers, test, D 2373 (06.03) iron content in paint driers, test, D3804 (06.03) lead content in paint driers, test, D 2374 (06.03) manganese content in paint driers, test, D 2375 (06.03) rare earths content (of paint driere) tet nu vanadium content in paint driers, U ]) zinc content in paint dners, test, D ton i<|<> M `T* zirconium content in paint driers, rein Efflorescence ^..' TM interior coatings (ofwater-base paint ni in , |tile/t I'solu prae' ip. co s See reporting paint film failures cbaracteustic ot ext paints, dassificatibn, D1848 (116.01) v Efflux cups '-jffl&L__ viscosity of paints/related materials, bv ISO 05125(06.03) ' Elasticity _ ,,,, elasticity/toughness of varnishes, test. 1) 1647 {06(01$ Electrical insulating solids r\ orange shellac/other indian lacs for electrical mrehrim D 784 (06t02) Mil shellac (dry/powdered) used for electrical irsuatSfii.it'' .test methods, D411 (06.02) `''.It ,*: Electrical measurements--coating applications 11 cathodic disbonding of pipeline coatings. aceeUraW test,, G 8 (06.01) ,i .-Jl*,; comparative corrosion preventive characteristics dfr used for joints/coupliflgs/fittings/pai clres m pipfci coatings, test,; G18 (06.01) ; ." A t- disbonding characteristics of pipehne coaiiniisubyidiiboi burial, test, G19 (06.01) ! ' discontinuity (holiday) testing of noncondnetive coating on metallic substrates, practic., D5t^(flftl<m [s,ter cef NJcohi effects of outdoor weathering on pipeline coat " { ii (06.oi) nAtamu impact resistance of pipeline coatings, hy u!hn*\uietikt G14 (06.01) impact resistance of pipeline coatings, bv limestone dfon G13 (06.01) water penetration into pipeline coatings, t.st G 9-(06.to Electrical stress >11' iVp ester) hy| lew |h#l cathodic disbonding of pipeline coatings, acedia,iwli'ifrc" test, G 8 (06(01) ; **111 Electrochemical measurements '_ nitrobenzene in aniline, test, D 4389 (06103. . Electrocoat baths .. . MwStr acid/base milliequivalent content of (anodic/calnudic)`!a 1 eiectrocoat baths/their ultrafiltcates, test, D 437flrt(tt analysis of eiectrocoat bath samples, guide, D (978 (06 ( apparent pH of eiectrocoat baths, test,.D 4584 (06.01)' electrical conductivity of eiectrocoat baths, test, D439|)i< nonvolatile and pigment content of eiectrocoat butlit,71^ muffle furnace, test, D 5145 (061)1) 'urtwiiSl Electrostatic spray ( yT' evaluating and comparing transfer conditions-lahoratorSJ. ,JK* conditions, test, D 5009 (06.01) ' 'J Electrostatic spray application testing industrial water-reducible coatings, guide, D 4712 (06.(1 Elongation mandrel bend test of attached organic coatings, test, D 522 (06.01) . ij`. Etli Elongation--attached organic coatings , elongation/tensile strength/stiffness, test, D 2370 (06 (11) Emergent stem temperature corrections distillation of industrial aromatic hydrocarbons, test, t :uKc*t 0 850(06.03) Emulsion vehicles (for paints/related coatings) blocking resistance of trade sales paints, test, D 4946 (06 Qlfcr? ^ freeze-thaw resistance of water-borne coatings, te t, * ;J u, , . D 2243 (06.01) i '| minimum film formation temperature (MEET) of omuls on vehicles, test, D 2354 (06.02) 1150 DUP050298326 Index of ASTM Standards, Section 6 Exposure tests- -carbon-arc apparatus ting industrial water-reducible coatings, guide, D 4712 (06.01) ' latile/nonvolatile content (of cellulosics/etnulsions/resin solutions/shellac/varnishes), selecting test procedures, practice, D 4209 (06.02) el coatings See Coatings--enamel h china clay See Aluminum silicate ride equivalent weight (EEW) oxy content of epoxy resins, test, D1652 (06.02) xy content .oxy resins, selecting test procedures, practice, D 4142 (06.02) itxy (EP) plastics--coatings objecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) pxy resins electing test procedures, practice, D 4142 (06.02) {librium method Sash point ofliquids, test, D 3941 (06.03) osion erosion testing of antifouling paints, using high velocity water, test, >4938(06.01) Exterior paints, method for evaluating, A D 662 (06.01) practical washability of organic coatings, tesb.D 4828 (06.01) jlwet abrasion resistance of interior paints to scrubbing, by weight loss, test, D4213 (06.01) ter content r I alcohol content/purity of acetate esters, by gas chromatography, test, DS3545 (06.03) Sters V-buty] acetate (all grades), spec., D 4615 (06.03) tester value of solvents and thinners, test; D1617 (06.03) ethyl acetate (all grades), spec., D 4614 (06.03) ' hexyl acetate, spec., D 5137 (06.03) f hydroxyl content of pyridine-soluble esters, by spectrophoto metry, test, A D 817 (06.02) ,! ' 5 isobutyi acetate (95 % grade), spec., D1718 (06.03) n-propyl acetate (96 % grade), spec., D 3130 (06.03) phthalic anhydride content- in presence of dibasic acids, by gravimetric test, T> 1306 (06.02) primary (synthetic) amyl acetate (98 % grade); spec., D 3540 (06.03) ter value ester value of solvents and thinners, test, D1617 (06.03) tching -- acid etching concrete, practice, D 4260 (06.01) heriiication sodium glycolate content of sodium carboxymethylcellulose, test, D 1439 (06.02) thoxy ethanol ` 2-ethoxyethanol, spec., D 331 (06.03) thoxyethyl acetate 2-cthoxyethyl acetate (99 % grade), spec., D3728 (06.03) alcohol content/purity of acetate esters, by gas chromatography, test, 0 3545(06.03) Ethoxyl content ethylcellulose, test, D 914 (06.02) Ethoxyl substitution ethoxyl substitution in cellulose ether products, by gas chromatography, test, D 4794 (06.02) Ethyl acetate alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) ethyl acetate (all grades), spec., D 4614 (06.03) (Ethyl acrylate ethyl acrylate (98.5 % grade), spec., D3548 (06.03) purity, by gas chromatography, test, D 3362 (06.03) Ethylbenzene aromatics (ethylbenzene and eight-carbon (C8/heavier) content in mineral spirits, by gas chromatography, test, 03257(06.03) ethylbenzene, spec., D 3193 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) purity of hydrocarbons from freezing points, test, D 1016 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D3437 (06.03) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) Ethylcellulose ethylcellulose, methods of testing, D 914 (06.02) Ethylenediamine tetraacetate (EDTA) content See EDTA method Ethylene glycol ethylene glycol, spec., D 2693 (06.03) glycerol/ethylene glycol/pentaerythritol in alkyd resins, test, D 1615 (06.02) Ethylene glycol monobnty) ether See Bntoxyethanoi Ethylene glycol monoethyl ether See Ethoxy ethanol Ethylene glycol monomethyl ether See Methoxy ethanol 2-Ethylhexanol 2-ethylhexanol (synthetic), spec., D 1969 (06.03) ethyl methyl pentanol content/purity value of 2-ethylhexanol, by gas chromatography, test, D 5008 (06.63) 2-Etbylhexyl acrylate 2-ethylhexyl acrylate, spec., D3541 (06.03) Ethyl iodide ethoxyl substitution in cellulose ether products, by gas chromatography, test, D 4794 (06.02) Ethyl methyl pentanol content ethyl methyl pentanol content/purity Value of 2-ethylhexanol, by gas chromatography, test, D 5008 (06.03) Ethyl silicate (inorganic) printer Sa Primer MEK resistance of ethyl silicate (inorganic) zinc-rich primers, 1 by solvent rub, test, D 4752 (06.01) Evaporation--rate/time volatile liquids with low viscosity, test, D3539 (06.01) Exempted solvents Sa Solvents (headings) -- dicbloromethane/1,1,1 -trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06.01) "v Expected flash point See Flash point (headings) Exposure--personnel design/use of safety alert system for hazardous work locations in coating/lining industry, practice, A D 4257 (06.01) Exposure tests freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, 0 2247 (06.01) water resistance of coatings, using controlled condensation, practice, D4585 (06.01) Exposure tests--carbon-arc apparatus accelerated testing of paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) carbon-arc light- and water-exposure apparatus, unfiltered, by Dew cycle, practice for operating, D 3361 (06.01) 1151 DUP050298327 Index of ASTM Standards, Section 6 Exposure tests- -carbon-arc apparatus /a'liiia conducting tests on paint/vamish/Iacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) operating carbon-arc light-exposure apparatus with and without water for exposure of nonmetallic materials, practice, G 23 (06.01) Exposure tests--corrosive environments evaluating filiform corrosion resistance of organic coatings on metal, test, D 2803 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D1654 (06.01), Exposure tests--exterior accelerated outdoor exposure tests ofcoatings (applied to metal substrates), practice, D 4141 (06.01) conducting exterior exposure tests of (exterior) paints on steel, test, D 1014 (06.01) conducting exterior exposure tests of house/trim paints on new/unpainted wood, practice, D 1006 (06.01) effects of outdoor weathering on pipeline coatings, test, G I I (06.01) quantifying dirt collection bn coated exterior panels, test, D 3719 (06.01) testing industrial water-reducible coatings, guide, D 4712 (06.01) Exposure tests--fluorescent-UV apparatus exposure of paints/related coatings to fluorescent UV- condensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) operating light-/water-exposure apparatus (fluorescent-UV condensation type) for exposure of nonmetallic materials, practice, G 53 (06.01) ' Exposure tests--light accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822(06.01) conducting tests on paint/vamish/lacquer/related products, . using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01); lightfastness of pigments (in artists' paints), test, D 4303 (06.01) lightfastness pf printed matter, D, 3424 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) operating light-/water-exposure apparatus (fluorescent-UV condensation type) for exposure of nonmetallic materials, practice, G 53 (06.01) Exposure tests--organic coatings detergent-resistance, practice, D 2248 (06.01) effect of chemical agents on organic finishes (used in transportation industry), practice, D1540 (06.01) effects of overbaking on organic coatings, practice, D 2454 (06.01) evaluating filiform corrosion resistance, test, I) 2803 (06.01) evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A D 2485 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D 1654 (06.01) recording results on single- and multi-panel forms, standard, AD 1150 (06.01) resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, D 3273 (06.01) testing finishes on primed metallic substrates for humidity-; thermai cycle cracking, D 2246 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D1735 (06.01) water resistance ofcoatings on steel, using water immersion, practice, D870 (06.01) wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Exposure tests--ultraviolet-cured coatings cure time, practice for reporting, D3',32 dio gii' estimating package stability of coattues fl ir ultra V Irt,Vn f&H test, D4144 (06.01) , Exposure tests--water erosion testing of antifouling paints, using high test, D 4938 (06.01) ` , -t V ' V S subjecting marine antifouling coating to la iuhifcife shear forces in natural seawater, test, 1)49)9 (O&Mr Exposure tests--xenon-arc apparatus ' '1 ` `1 j *"' operating light-exposure apparatus (Xenon-nre without water for exposure of noun ajllic m practice, G 26 (06)01) - Extender pigments \ Scf, AluniinumSilicate/Bariumsuliati i'.il,Jni ' earbonate/Cblcium sulfate Magnesium silicate ' vJS _ Silica (diatomaceous)011 * ^ $3^^$ particle size distribution, by hydrometer of com non,juju extender pigments, test, D 3360 (06.02) /'Ji . yellow/orange/greeirpigmentscontaining!-.J rijomai chromium oxide green, analysis test,]) 126 ({fcj)2} Exterior durability See Durability . ... * isJaaihsiiE ` "'-'l Exterior paints/coatings -i j }i conducting exterior exposure tests of bou>u/mjtetnaj&3 new/unpainted wood, practice. D 1006 lOd.fluSxrjfo degree of checking, evaluation, test. A I) 660 " degree ofcracking evaluation, test, A I) 661 l08UUf degree of erosion, evaluation, A 1)662 (flh.im " '* degree of flaking, evaluation;,A D772 (0611J) i, house and trim coatings; solvent-based praeticcsiLg selecting/using testprocedures, pijcttu.DjSSZ1? latex house painls, selecting/using test proc -dupes, 8i ` D3129 (06.01) quantifying dirt collection on coated extern u MnJiir'S D 3719(06.01) . .,-^35 reporting paint Elm failures characteristicof paints, classification, D1848 (06,01) testing solvent-borne architectural (interior, eve .oiKi guide, D 5146 (06,01) testing water resistance of coatings at 100 feifelffilpp practice, D 2247 (06.01) Extraetion.'methpds , ->.- unsaponifiable matter content of rosin, test 1) 1065 ( Extractives content dichloromethane-soluble matter content of cel'mlosi D3971 (0-3.02) Cyf Fabrication ' ' design/fabrication of flue gas desulfurization ' ysteni'So'ijijSL _ (fbr protective lining application), spec , D 4ol8<^l)ftjH^g^fW| profile of abrasive blast-cleahed steel surfarcs, in fbrirai . field/fabricating shop, test, D 4417 (06.01) ' * .jup ^ Face glazing and bedding compounds--metal sash * <o-J slump of face glazing/bedding compounds on in.Ul sash, jafi* ;i* D 2376 (06.01) , Factory-applied organic coatings See Organic coatings ,r1J 45- Failure end point . . .....................M photographic documentation of coatings/liningi cctects; failures, D 4121 (06.01) pull-off strength ofcoatings,' using portable atiiusion 4 test, D 4541 (06.01) '< reporting paint film failures characteristic of csle-ii r lawx^- paints, classification, D1848 (06.01) * '* 4. 1 1152 Falii I iiri allii ir im. jpattj fat ' fat id$ r Fatty* aTt* fefe i Fatt; to "Mtiii DUP050298328 U. hv:4| w * Cl Index of ASTM Standards, Section 6 Fiber-optic light j rod viscometer (viscosity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) ping sand abrasion test ' brasion resistance of organic coatings, by falling abrasive, test, D 968 (06.01) Bing stones npact resistance of pipeline coatings, by limestone drop test, G13 (06.01) ,, lling weight test Ipnpact resistance of pipeline coatings, by felling weight test, G14 (06.01) _^nt ,.v Besting industrial water-reducible coatings, guide, D 4712 (06.01) Jitty acids--general (fatty acid composition, by gas-liquid chromatography of methyl I esters, test, D1983 (06.03) (fetty acids used in protective coatings--terminology mid | selecting test methods, guide, D 1467 (06.03) f identification of oils and oil acids in solvent-reducible paints, test P 2245 (06,03) || preparation of methyl esters from fatty acids, for fatty acid composition analysis, test, D 3457 (06.03) (sampling liquid oils/fatty acids (commonly used in paints/ vamishes/related materials), test, D1466 (06.03) Batty acids--specifications 1 coconut oil, spec., D1841 (06.03) B corn oil, spec,, D1842 (06.03) i cottonseed oil, spec., D1843 (06.03) dehydrated castor oil, spec., D 1539 (06.03) J linseed oil, spec., D1538 (06.03) 1 soybean oil, spec., D1537 (06.03) jfsM oil,1 spec., D1984 (06.03) atty acids--tests B acid value of fatty acids/polymerized fatty acids, test, D1980 (06.03) ash content, test, D1951 (06.03) clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) color after heating, test, D1981 (06.03) color of transparent liquids, by Gardner color scale, test, D1544 (06.01,06.02,06*03) fatty acids used in protective coatings--terminology and selecting test methods, guide, D 1467 (06.03) fish oil content, by gas-liquid chromatography, test, D 3725 (06.03) hydroxy) value of fetty oils/acids, test, D1957 (06.03) iodine value, test, D 1959 (06.03) polymerized fatty acids, selecting test methods, D 2575 (06.03) rosin acid content, test, D 1240 (06.03) saponification value ofdrying oils/fatty acids/polymerized fatty, acids, test, D1962 (06.03) solidification (titer) point of fatty acids/test, D1982 (06.03) specific gravity at 25/25C, test, D 1963 (06.03) unsaponjfiable matter in drying oils/fatty acids/polymerized fetty acids, test, D 1965 (06.b3) [fFatty acids content alkyd resins and alkyd resin solutions, test, D 1398 (06.02) fatty acid composition, by gas-liquid chromatography of methyl esters, test, D 1983 (06.03) oleic acid content of tall oil rosin, test, D1585 (06.03) preparation of methyl esters from fatty acids, for fatty acid composition analysis, test, D 3457 (06.03) tall oil, methods of testing, D 803 (06.03) | Fatty amidoamines fatty nitrogen compounds, selection of test methods, D 2071 (06.03) iodine value, by Wijs procedure, test, D 2075 (06.03) total/primary/secondary/tertiary amine values of fatty amines/amidoamines/diamines, by referee potehtiometric method, test, D 2073 (06.03) water content, test. D 2072 (06.03) Fatty amines fatty nitrogen compounds, selection of test methods, D2071 (06,03) iodine value, by Wijs procedure, test, D 2075 (06.03) non-amine component content of fetty amines/nohamines, test, D 2082 (06.03) percent of amines (primary/seeondary/tertiary) in fatty amines, test, D 2083 (06.03) total/primary/secondary/tertiary amine values of fatty amines/amidoamines/diamines, by referee potentiometric method, test, D 2073 (06.03) total/primary/secondary/teitiary amine values of fatty amines, by alternative indicator method, test, D 2074 (06.03) water content, test, D 2072 (06.03) Fatty diamines fetty nitrogen compounds, selection of test methods, D 2071 (06.03) iodine value, by Wijs procedure, test, D 2075 (06.03) non-amine component content of fatty amines/bonamines, test, D 2082 (06.03) total/primary/secondary/tertiary amine values of fatty amines/amidoamines/diamines, by refetee potentiometric method, test, D 2073 (06.03) water content, test, D 2072 (06.03) Fatty matter content sampling/testing flaked aluminum powders/pastes, methods, D 480 (06.03) Fatty nitrogen compounds identification of oils and oil acids in solvent-reducible paints, test D 2245 (06.03) non-amine component content of fatty amines/nonamines, test, D 2082 (06.03) selection of test methods, D 2071 (06.03) water content, test, D 2072 (06.03) Fatty quaternary ammonium chlorides acid/amine value of fatty quaternary ammonium chlorides, test, D 2076 (06.03) ash content, test, D 2077 (06.03) average molecular weight determination, test, D 2080 (06.03) fatty nitrogen compounds, selection of test methods, D 2071 (06.03) iodine value, test, D 2078 (06.03) nonvolatile matter (solids) content, test, D2079 (06.03) pH, test, D 2081 (06.03) water content, test, D 2072 (06.03) Federal Standards index of ASTM methods equivalent/related to methods in Federal Standard 141 ("(feint, Varhish, Lacquer, and Related Materials; Methods for Sampling and Testing"), (Related Material).(06.01,06.02, 06.03) Feedstock xylenes for p-xylene feedstock, spec., D 5211 (06.03) Ferric chloride methylol group determination (qualitative) in phenolic resins, test, D 4706 (06.02) Ferric oxide Sa Iron oxide pigments ferric oxide in barium sulfate pigment, test, D 715 (06.02) Ferrite pigments See Iron oxide black - Ferrous iron content iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) Ferrous sulfate titration nitrogen content of soluble nitrocellulose, by ferrous sulfate procedure, test, D 4795 (06.02) Fiber-optic light See Light--transmission and reflection 1153 DUP0502 98329 Index of ASTM Standards, Section 6 Fibrous magnesium silicate Fibrous magnesium silicate See Magnesium silicate Field testing--`paints/related coatings/materials assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) , conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) conducting a patch test to assess coating compatibility, practice, D 5064 (06.01) field identification of coatings, test, D 5043 (06.01) ,, profile of abrasive blast-cleaned steel surfaces; in laboratory/ field/fabricating shop, test, D 4417 (06;01) Filiform corrosion resistance Sa Corrosion (headings) organic coatings on metal, test, D 2803 (06.01) Film exposure of paints/related coatings to fluorescent UV- condensation light-water-exposure apparatus, practice for conducting tests, D4587 (06.01) film hardness (of factory-applied organic coatings on metal substrates), by pencil test, D3363 (06.01) * mandrel bend test of attached organic coatings, test, D 522 (06.01) i preparation of free films of organic coatings, practice, D4708 (06.01) preparing drawdowns of artists' paste paints, practice, D4941 (06.01) .; producing films of uniform thickness of paint/varnish/related products on test panels, test, D 823 (06.01) . . ;< reporting paint film failures characteristic of exterior latex, . paints, classification, D 1848 (06.01) Film--dry film thickness , coatings on wood products, methods for microscopical measurement, D 2691 (06.01) coil coatings, application using a wire-wound drawdown bar, practice, D 4147 (06.01) dry film thickness of nonconductive coating? (applied to rionferrous metal base), nondestructive measurement, test, D 1400 (06.01) dry-film thickness of organic coatings, rising micrometers, test, D1005 (06101) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) erosion testing of antifouling paints, using high velocity water test, 0 4938(06.01) film thickness of pipeline coatings op steel, nondestructive measurement, method, G 12 (06.01) nonmagnetic coatings (paint/vamish/lacquer), applied to a ferrous base, D1186 (06.01) , penetration resistance of pipeline coatings, by blunt raid test, G 17 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) Film--electrical conductors soluble cellulose nitrate, testing, methods, D 301 (06.02) Film--formation'rates minimum film formation temperature (MFFT) of emulsion vehicles, test, D 2354 (06.02) organic coatings (at room temperature), test, D 1640 (06.01) testing industrial water-reducible coatings, guide, D4712 (06.01) Film--wet film thickness wet film thickness of organic coatings, D 1212 (06.01) Film failure See Failure end point (headings) Filter-retained solids filter-retained solids content of polymer latexes, test, D 5097 (06.02) Fineness reporting particle size characteristics of pigments, practice, 01366(06.02) Fineness of grind (dispersion) , yj fineness of dispersion of pigment-vehii t -wuenis * D 1210 (06.01) ' ' r! priming inks, by NPIRI method, test, D 131<i (do (j 1 Finger-rub test field identification of coatings, test, D S043 (0601) Finite closed-cup flash point methods See Flash point (headings) n Fire retardancy *T See Fire testing--fire/flame retardancy t -,f} Fire testing--ptiints/related coatings/materials fire retardancy of paints, by cabinet method, test AD 1360 (06.01) ` , flash/fire point dfliqtfitis, by Tag open-cup apparatus test D 1310 (06.03) ,,-,j,, stnaU-sealefievaluation of fire-retardant paints: by 2-Jo-t tunnel method, test, D 3806 (06.01) sustained bunting (of liquid mixtures),"by Seta-flSSh tutu-, tAnenH cup), test; D 4206 (06,01,06.03) ( s. . j sustained bunting (Of low viscosity liquid mixtures . h wfi-gr# test, D 4207 (06.03) 'kV Fire testing--jtetroleum'prpducts :1 flash/fire point,ofliquids; by Tag'dpenteupapparatiis, D1310 (06.03) ' ' First aid handling/sampling phenol and cresylic acid, practice, r D 3852 (06.03) ' ' it-l'.. sampling and handling aniline, practice, D 3436 (U603)!l Fischer reagent method (for wptcr content) See Karl Fisciier reagent method ,, j Fish oil content S fish oil content of drying oils and their fatty acids, hy pas- iquid " chromatography, test, D 3725 (06.03) Fittings comparative corrosion preventive characteristics.pf mulct) used for joints/couplings/fittings/patches in pipeline coatings, test, G 18 (06,01) Five-degree xy.lene/5q xylol . See Xylene (five-degree) , , Fixed alignment adhesion tester -1 pull-off strength of coatings, using portable adhesion-testers, ~3jj test; 04541 (06.01) , .. , ,T J Flake brass . See Copper powder/GoId bronze powder ' Flaked powders sampling/testing flaked aluminum powders/pastes.,'methods, * , D 480 (06.03) * ' f- Flake white "~ / ` J ^' See Basic carbonate white lead 'J FlaRilig ' exteriorjpainis, A D 772 (06.0.1) , Flame cleaning standard pictorial surface preparation standards for painting steel surfaces, A D 2200 (Q6,01) . Flame photometric detectors (FPD) thiophene-content of refined benzene, by gas chromatography (with flame photometric detection), test, D 4735 .(06.03) Flame spread small-scale evaluation of,fire-retardant paints, by 2-foot tunnel- method, test, D 3806 (06,01) t Flammability--paints/relafed coatings/materiais fire retardancy of paints, by cabinet method, test, A D 1360 (06.01) flash/fire point of liquids, by Tag open-cup apparatus, test, D 1310 (06.03) small-scale' evaluation of fire-retardant paints, by 2-foot tunnel method, test, D 3806 (06.01) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D 4206 (06.01, 06.03) 1154 DU PO50298330 Index of ASTM Standards, Section 6 Fungal influence- -paints/related coatings/materials istained burning (of low viscosity liquid mixtures), by Wick test, D 4207X06.03) notability1--petroleum products ish/fire point of liquids, by Tag open-cup apparatus, test, 0-1310 (06.03) h/no flash method mpliance by liquids of closed-cup flash point specifications, D 3934 (06.03) : Ph print--liquids . IquUibjrium method, test, P 39,<|i (06,0,3) , Oash/fife point ofliquids, by Tag openrcup apparatus, test, D1310 (06.03) ijlash/no flash equilibrium method, D 3934 (06.03) Bash point by Tag closed tester, list, D 5fi (06,03) V "isii point '(of fuel oils/liibe oils/suspension of soUds/liquids), by ,, Pensky-Martens ciosed tester, test, D 93 (06.03) (flash point ofliquids, BySetaflash dosed-cup apparatus, test, I D3278 (06.03) feustained burning (of liquid mixtures), by Seta-flash tester (open I cup), test, D*4206 (0S.pl, 06.03) pusfained'`hainfng (of lbiv yiscosity liquid mixtures), by Wick I test, D 4207 (06.03) fital bil/methods of testing, D 803 (06.03) Bat interior Jlatesx paint * (See .Latex paints ' mandrel bend test of attached organic coatings, test, | D 522 (06.01) | organic coatings, (paints) on prepainted deformed metallic sheets, test, D 4145 (06.01) dear floor sealers, performance tests, O 1546 (06-01) 'f solvent-thinned paints, practice for selection and use of test procedures, D 3383 (06.01) ,' ; water-thinned floor paints, selection and uSq of test procedures, practice, D 3358 (06.01) |low and flow rate--paints/related coatings/materials 1 high sh,ear yiscosity (ofpgints/varnishes/related products), by 1CI cone/plate viscometer, test, D 4287 (06.01) i shellac (dry/powdered) used for electrical insulation, selecting test methods, D 411 (06.02) , testing industrial water-redudble coatings, guide, D 4712 (06.01) viscosity of paints/related materials, by ISO flow cups, test, D 5125 (06.03) ^owcoat testing industrial water-reducible coatings, guide*, D 4712 (06.01) 'low cup viscosity of paints/related materials, by ISO flow cups, test, D 5125 (06.03) viscosity of paints/varnishes/lacquers, by Ford viscosity cup* test, D1200 (06.01) Flue gas desulfurization system design/fabrication (for protective lining application), spec., D 4618 (06,01) jjFluorescent UV-condensation apparatus exposure of paints/reiated coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) operating Iight-/water-exposure apparatus (fluorescent-UV , condensation type) for exposure, of nonmetallic materials, practice, G 53 (06.01) fFoil film thickness of pipeline coatings on steel, nondestructive measurement, method, G 12 (06.01) |Foots .1 d foots in raw linseed oil, by gravimetric method, test, D 1966 (06.03) foots in raw linseed oil, by volumetric method, test, D 1954 (06.03) Ford cup viscosity of paints/varnishes/lacquers, by Ford viscosity cup, test, D 1200 (06.01) Ford viscometers See Viscometers--Ford Foreign matter content clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) Formability factory-applied, organic coatings on metal substrates, by Impact-Type Wedge Bend test; D 3281 (06.01) formability/adhesion of zinc-rich primer/chromate complex coatings (on steel), test, D 4146 (06.01) Formaldehyde acidity, test, D 2379 (06.03) - concentration bf formaldehyde solutions, test, D 2194 (06.03) formaldehyde- 50 % grade (unhibited) and 37 % grade (inhibited/uiihibited), spec., D 2378 (06,03) free formaldehyde content ofamino resins, test, D 1979 (06.02) iron content, test, D 2087 (06.03) methanol content of formaldehyde solutions, test, D 2380 (06.03) Formic acid content glacial acetic acid, method, D 3546 (06.03) Forms for exposure tests See Records management Formulation data calculating formulation physical constants of paints/coatings, practice, D5201 (06.01) Fractionated and distilled fatty acids See Fatty acids--specifications Free formaldehyde See Formaldehyde Free monomers unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) Free phenols See Phenol Free silica content See Silica content Free toluene diisocyanate content urethane prepolymers/coating solutions, by gas chromatography, test, D3432 (06.02) Freezing and thawing--resistance freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) freeze-thaw stability of multicolor lacquers, test, D 2337 (06.01) Freezing point freezing points of high-purity hydrocarbons, test, D. 1015 (06.03) purity of hydrocarbons from freezing points, test, D1016 (06.03) purity of styrene, by freezing point method, test, D 3799 (06.03) French blue See Iron blue French chalk ' See Magnesium silicate French ocher See Ocher Fresnel reflector rack exposure method accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D4141 (06.01) Friction/frictibhaf properties static friction of coating surfaces, test, D 4518 (06.01) Fuel resistance solvent/fuel resistance of traffic paint, test, D 2792 (06.01) Fungal influence--paints/related coatings/materials paint films, evaluating degree of surface disfigurement, A D 3274 (06.01) 1155 DUPO 50298331 Index of ASTM Standards, Section 6 Fungal influence--paints/related coatings/materials presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, D 3273 (06.01) Fungicidal pigments See Calcium borosilicate/Zinc oxide Furnace black See Carbon black (headings) Furnaces chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium,dioxide, test, D 4797 (06.01) nonvolatile and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (06.01) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D 4451 (06,01) Furniture finishes temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D1211 (06.01) G GA-CAT comprehensive abrasion test abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) Gages wet film thickness of organic coatings, by notched gages, practice, D 4414 (06.01) Galvanized surfaces See Steel panels/Steel pipe/tube/Steel sheet Gamma radiation effects of radiation on coatings (for light-water nuclear power plants), test, D 4082 (06.01) Gardner-Coleman method , oil absorption of pigments, test, D 1483 (06.02) Gardner color scale color of transparent liquids, by Gardner color scale, test, D1544 (06.01, 06.02,06.03) Gardner-Holdt viscometers See Viscometers--Gardner-Holdt Garnet lac orange shellac and (button lac/garnet lac), spec., D 237 (06.02) sampling/testing lac resins (orange shellac/button lac/garriet lac/bleached lac), test, D 29 (06.02) Gas black pigment See, Pigments--carbon black . Gas checking draft test varnish films, test, D 1643 (06.01) Gas chromatography See Chromatography--gas (headings) Gelled vehicle laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) Gel time drying oils, test, D 1955 (06.03) tar acids, test, D 2870 (06.03) Generic resin field identification of coalings, test, D5043 (06.01) Glacial acetic acid formic add in glacial acetic add, test, D 3546 (06.03) glacial (99.8 %) acetic acid (for use in paint/varnish) lacquer/related products), spec., D 3620 (06.03) Glacial acrylic acid See Acrylic acid Glacial methacrylic acid See Methacrylic acid (glacial) Glass panel reading surface wet film thickness of organic coatings, D 1212 (06.01)' Glass panels directional reflectance factor (45-deg 0-de_) of opacituM- specimens, by broad-band filter rsfleLCcmcln r.'.r E97 (06.()1) 1 surface preparation (for testing paints, varnish laam,TM- i-i' coatings), D 3891 (06.01) .wcquur & re Glass spheres (in traffic paint/marking material) chemical/gravimetric analysis of white/yellow th traffic marking material containing lead i' titanium dioxide, test, D 4797 (06.01) sieve analysis of glass spheres (for retrorefioctive markings/industrial uses), test, D1214 (Q6.02) test for roundness of, D 1155 (06.02) ' * `' Glazing compounds--metal sash slump of face glazing,'beddiog compounds on metal vacTh D 2376 (06.01) ^ viscosity of printing inks/vehides, by faHing-iod visco-n?t**r test, D 4040 (06.01) ', H1 Gloss ' -1 clear/pigmented organic coatings, test, D1308 (06 0J) gloss differences between,surfaces of similar apleararae ' v for visual evaluation, D 4449 (06.01) ,, gloss of high-glosstmetaUic/nonmetallic surfaces, bv liomon1 metry, method, E 430 (06.01) ***""* gloss/sheen uniformity evaluation, test, D 3928 (06.01) practical washability of organic coatings, test, D 4828 (06Jli') reflection haze of high gloss surfaces, test, D 4039 106.01)' specular gloss of nohmetallic specimens, test, D 52) (06JnH*-"f. Gloss paints 4fe interior latex semigloss/gloss paints, 'selecting test trctl.ud? !if5' 5? guide, D 4540 (06.01) GIne gas desulfurization (FGD) inspection of linings in operating flue gas desulf in/.tnonV^'i,V systems, practice, D 4619 (06.01) Glycerin--high-gravity ; high-gravity glycerin', spec., D1257 (06.03) sampling/testing high-gravity glycerin, test, D1258 (06.03 Glycerol and ethylene glycol content ' glycerol/ethylene glycol/pentaerythritol in alkyd nuns, t D1615 (06.02) Glyddyl ethers total chlorine content in epoxy resins/compbunds, test, D 4301 (06.02) Glycol ethers h purity of propylene glycol monomethyl ether/dipropyfincfgb monomethyl ether/propylene glycol monomcthy, tthi.r'*' acetate, test, D4773 (06.03) Glycols ~~ See Engine coolants Gold bronze powder ' '* chemical analysis of cuprous oxide/copper pigments, test, *( D 283 (06.02) gold bronze powder, spec., D 267 (06.02) Government specification fire retardancy of paints, by cabinet method, tesi A D1360 (06.01) Grading sampling/grading rosin (delivered in commercial bags/ > barrels/drums), test, D 509 (06.03) Graphics ' abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) Graphitic mica See Stone--mica Gravimetric method resin solution dilutability, test, D 5062 (06.03) !Sd' water pickup of lithographic printing inks/vehicles m a laboratory mixer, test, D 4942 (06.01) white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) 1156 DUP050298332 Index of ASTM Standards, Section 6 Heating tests--paints/related coatings/materials Ireen pigments |, Sa Chrome green/Chromium oxide green I Phthalocyanine green f yellow/orange/green pigments containing lead chromate/ | chromium oxide green, analysis, test, D126 (06.02) pipd (pigments) I? See Fineness of grind (dispersion) p I filter-retained solids content of polymer latexes, test, I; 0 5097(06.02) grit content I grit content of mica pigment, test, D 716 (06.02) Iround dolomite/limestone/oyster shell '$ See Calcium carbonate Snides for testing paints/related coatings/materials alkyd resins, practice, D 2689 (06.02) !; amino resins, selecting test procedures, practice, D 4277 (06.02) 1 analysis ofelcctfocoat bath samples, guide, D1978 (06.01) I architectural paints/coatings (soivent-/water-thinned), ! D 2833 (06.01) chemical analysis of white pigments, selection of test methods, guide, D 34 (06.02) clear/pigmented lacquers, D 333 (06.01) coil coatings, testing, practice, D 3794 (06.01) drying oils, selecting "test methods, guide, D 555 (06.03) epoxy resins, selecting test procedures, practice, D 4142 (06.02) evaluation of (clear/pigmented) coatings for rigid/semirigid plastic substrates, practice, D 3002 (06.01) ' exterior latex house paints, practice, D 3129 (06.01) exterior solvent-based house/trim coatings, practice, D 2932 (06.01) fatty acids used in protective coatings--terminology and .. selecting test methods, guide, D1467 (06.03) fatty nitrogen products, D 2071 (06.03) floor paints (solvent-thinned), practice, D 3383 (06.01) , floor paints (water-thinned), practice, 0 3358 (06.01) interior flat wall paints (latex), practice, D 2931 (06.01) interior flat wall paints (solvent-thinned), practice, 03323(06.01) interior latex semigloss/gloss paints, selecting test methods, guide, D 4540 (06.01) interior semigloss wall/trim enamels (Solvent-thinned), practice, D 3425 (06.01) latex vehicles, selecting test procedures, practice, 04143 (06.02) nonvolatile matter content (of paint/raw paint materials), practice, D 2832 (06.01) polymeric pawders/powder coatings, practice, D3451 (06.01) polymerized fatty acids, selecting test methods, D 2575 (06.03) polyCvinyl chloride) resins, guide, D 4368 (06.02)' printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) sampliog/testing volatile solvents/chemical intermediates (for paints/lacquer/vamish/related material), selecting test methods, D 268 (06.03) testing industrial water-reducible coatings, guide, D4712 (06.01) testing primers/primer surfacers over preformed metal, 1 selection/use of procedures, practice, D 3322 (06.01) traffic paints, practice, 02205 (06.01) " traffic paint, uniformity ofvehicle solids, by spectroscopy/gas chromatography, practice, D 2743 (06.01) varnish, D154 (06.01) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, 04209 (06.02) volatile/nonvolatile content (of driers/drying oils/naval stores and. solvents), selecting test procedures, guide, D 4140 (06.03) volatile/nonvolatile content (of pigments), selecting test procedures, guide, D 4139 (06.02) volatile organic content (VOC) of paints/related coatings, selecting test procedures, practice, D 3960 (06.01) Gum content artists' paints (oii/resin-oil/alkyd), spec., D 4302 (06.01) Gum rosin See Rosin Gum spirits of turpentine See Turpentine H Halo-silane coated glass plates preparation of free films of organic coatings, practice, D 4708 (06.01) Halphen-Hicks test qualitative detection of rosin in varnishes, by LiebermanStorch/HaSphen-Hicks tests, D 1542 (06.01, 06.02) ' Handling materials See Material handling Hardness (indentation) indentation hardness of organic coatings, by Knoop and Pfund methods, test, D1474 (06.01) Hardness tests--organic coatings film hardness, by pencil test, D 33.63 (06.01) hardness of organic coatihgs, by Konig/Persoz pendulum hardness tests, D4366 (06.01) indentation hardness oforganic coatings, by Knoop and Pfund methods, test, D1474 (06.01) Hazardous constituents analytical procedures for determining hazardous constituents in protective coatings, selecting test methods, guide, D 3630 (06.01) Hazard potential--health analytical procedures for determining hazardous constituents in protective coatings, selecting test methods, guide, D 3630 (06.01) design/uSe of safety alert system for hazardous work locations in coating/lining industry, practice, A D 4257 (06.01) handling cresylic add and phenol, practice, 03852 (06.03) handling naphthalene, maleic/phthalic anhydride, practice, 0 3438(06.03) labeling art materials for chronic health hazards, practice, D 4236 (06.01) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, 0 4297 (06.03) Haze Sa Gloss cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, 0 87X (06.02). gloss of high-gloss metallic/nonmetaliic surfaces, by goniophoto- metry, method, E 430 (06.01) reflection haze (of high gloss surfaces), test, 0 4039 (06.01) Heat and flame response See Flash point (headings) Heat-bodied drying oils acetone tolerance of heat-bodied drying oils, test, D1950 (06.03) Heated black box exposure test accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, 04141 (06.01) Heating tests--paints/related coatings/materials cellulose acetate propionates/butyrate, test, A D 817 (06.02) chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) distillation of industrial aromatic hydrocarbons/related materials, method, 0 850 (06.03) evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A 0 2485 (06.01) loss on heating of drying oils, test, D 1960 (06.03) 1157 DU P050298333 Index of ASTM Standards, Section 6 Heating tests- -paints/related coatings/materials ins m stroke cure time of thermosetting phenol-formaldehyde resins, test, D 4640 (06.02) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D 4206 (06.01, 06.03) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) temperature-change (high-low) resistance of dear nitrocellulose lacquer films applied to wood, test, D 1211 (06.01) water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) Heatset-type printing inks nonvolatile content of printing inks/resin solutions/vehicles, test, D 4713 (06.01) Heavy metals lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) Heavy metals content hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) methylcellulose, test, D 1347 (06,02) Hegman scale fineness of dispersion of pigment-vehicle systems, test, D 1210 (06.01) Hematite See Iron oxide red n-Heptane flash/fire point ofliquids, by Tag open-cup apparatus, test, D1310 (06.03) heptane miscibility of lacquer solvents, test, D1476 (06.03) purity of hydrocarbons from freezing points, test, P 1016 (06,03) Heptane miscibility Sa Miscibility heptane miscibility of lacquer solvents, test, D1476 (Q6.03) Herring content fish oil coutent (of drying oils and their fatty acids), by gas-liquid chromatography, test, D 3725 (06.03) n-Hexane purity of hydrocarbons from freezing points, test, D 1016 (06.03) Hexanes commercial hexanes, spec.', D1836 (06.03) Hexyl acetate hexyl acetate, spec., D 5137 (06.03) Hexylene glycol ' hexylene glycol, spec., D 2636 (06.03), Hiding power hiding power of architectural paints applied by roller, test, D 5150 (06.01) Hiding power--paints/coatings comparison of the brush drag of latex paints, test, D 4958 (06.01) hiding power of paints, by reflcctometry, test, A D 2805 (06,01) relative dry hiding power, D 344 (06.0)) wet-to-dry hiding change of architectural coatings, test, D 5007 (06.01) High-flash aromatic naphthas See Naphtha and naphtha derivatives High-gravity glycerin See Glycerin--high-gravity High-purity water reagent water, spec., D1193 (06.03) High resilience polyurethane foam See Urethanes--foam High shear viscosity comparison of the brush drag of latex paints, test, D 4958 (06.01) High-speed centrifugal vehicle separations See Vehicle separation - High velocity water >' i erosion testing of antifouling paints usirte to h test, D 4938 (06.01) "' High voltage continuity testing continuity verification of liquid/sheet itnin.w oj, substrates, practice, D 4787 (06111) " , High voltage spark testing " 1 , discontinuity (holiday) testing of noncondu, r, proWw? , coating on metallic substrates, pr,,.D $l6r<ptfjfjrfa Holiday detection `A cathodic disbonding of pipeline coatinEs'Jccefelniic?,. test, G 8 (06.01) continuity verification of liquid/sheet lining appli'jijC' substrates, practice, D 4787 (06.01)' r disbonding characteristics of pipeline coatings, te HiW-tfo burial, test, G 19(06,01) ` /-sgs discontinuity (holiday) testing of nonconductor kteS* coating on metallic substrates, practice, n 5tfi2 ?M(Tj i impact resistance ofpipeline coatings, by lime-topc.rfrm.r'stf' G13 (06.01) Horizontal pnll test . ' TnRnfin static friction of coating surfaces, test, D 4M8 (0601.) j* 4l,CK Humidity l-ZmmBm humid-dry cycling for coatings on wood/jwo rd prodyctV!'^'' method, D 3459 (06.01) '. r,` ?**<**.. humidity-thermal cycle cracking, testing finishes ouxfb&'-'-'J'S *'S surfaces, D 2246 (06.01) . Humidity--relative w testing water resistance of coatings at 100 % relate practice, D 2247 (06.01) Hunter appearance gloss differences between surfaces of similar Pt-evatfcvV^- for visual evaluation, D4449 (06.01) Hydrated iron oxide * *#f ! ochre pigment, spec., D 85 (06.02) . Hydrocarbon content--nonaromatic total non-aromatic/trace monocyclic hydepe " bon aronjtjJtd' xylene D 2306 (06.03) Hydrocarbons acidity ..."....... " MM benzene content of cyclic hydrocarbon products, b> gat .i`i>Tt3-a chromatography, test, D 4534 (06.03) ', dichloromethane/l,l,l-trichloroethane content in paints/ s.,'* coatings, by direct injection gas cbrom.ungraphy test,' ' >7 , , D 4457 (06.01) high-flash aromatic naphthas, spec., D 3734 (06.03) . vt mineral (petroleum) spirits hydrocarbon dr.cic.1nn3 solvent,', -< J . spec., D 235 (06.03) . sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) 1 unreacted monomer content of latexes, by gas-hquid chromatography, test, D 4747 (06.02) VM & P naphthas, spec.. D 3735 (06.03) Hydrocarbons--aromatic aromatic hydrocarbons/related chemicals, terminology 0 4790(06.03) bromine content, by coulmetric titration, test, D1492 (06.03> color (of solid aromatic hydrocarbons/relatcd materials "in' molten state), by platinum-cobalt'scale, tests D 1686 (06.03) ' solidification point of 4,4- isopropyhdenediphenol (Bismonol A), test, D 4493 (06.03) |ydroi ; acid . |;Hyir vbl 1158 jt **,.- DUP050298334 Index of ASTM Standards, Section 6 Industrial aromatic hydrocarbons al non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, by gas chromatography, test, D 2360 (06.03) ce (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06.03) ocarbons--high-puritv ' mercial density (of pure liquid chemicals), test, D 3505 (06.03) "ing points of high-purity hydrocarbons, test, D1015 (06.03) rity of hydrocarbons from freezing points, test, j D1016 (06.03) lidification point of industrial organic chemicals, test, D1493 (063)3) carbons--industrial aromatic < 'dity of benzene/toluene/xylenes/solvent naphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) id wash color, test, D 848 (06.03) pparent density of industrial aromatic hydrocarbons, test, ` D 2935 (06.03) pmmereial density (of pure liquid chemicals), test, D 3505 (06.03) popper corrosion of industrial aromatic hydrocarbons, test, ' D 849 (06.03) istiliation, test, D 850 (06.03) ydrogen sulfide and sulfur dioxide content (qualitative), test, C D 853 (06.03) olidification point of industrial organic chemicals, test, D1493 (06.03) lfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, D3961 (06.03) Ivolume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) drocarbons--tight volume/weight of industrial aromatic hydrocarbons, method, D 1555 (06.03) 'drodynamic stress subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) ydrogen sulfide content i:industrial aromatic hydrocarbons, test, D 853 (06.03) ydrolyzable chlorine content hydrolyzable chlorine content of liquid epoxy resins, test, D1726 (06.02) ydroquinone content hydroquinone in vinyl acetate, test, D 2193 (06.03) ydroxyacetone content | analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, 0 4961(06.03) ,f ydroxyethylcellulose f hydroxyethylcellulose, test, D 2364 (06.02) ydroxyl (hydroxide ion) content f hydroxyl content of cellulose acetate, by spectrophotometry, test, D 871 (06.02) hydroxyl content of pyridine-soluble cellulose esters, by spectrophotometry, test, A D 817 (06.02) hydroxyl value of fatty oils/acids, test, D 1957 (06.03) ; pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) lydroxypropoxyl content hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) Hydroxypropyl methylceilutose hydrogen sulfide/sulfur dioxide (qualititative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) hydroxypropyl substitution methoxyl/hydroxypropyl substitution in cellulose ether products, by Zeisel-gas chromatography, test, D 3876 (06.02) Hygroscopic materials/properties/tests hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, D 280 (06.02) water content in phenol/related materials, by iodine reagent method, test, D 1631 (06.03) I ICI cone/plate viscometer high shear viscosity (of paints/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Identification field identification of coatings, test, D 5043 (06,01) Ignition--loss on ignition . moisture content of pigments, D1208 (06.02) Ignition residues of drying oils See Ash content Immersion chemical resistance of pipeline coatings, test, G 20 (06.01) comparative corrosion preventive characteristics of materials used for joints/couplings/fittmgs/patches in pipeline coatings, test, G 18 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) Impact testing--pipeline coatings effects of outdoor weathering on pipeline coatings, test, Gil (06.01) impact resistance of pipeline coatings, by falling weight test, G14 (06.01) impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) Impressed current system cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) Imprinting print resistance of architectural paints, test, D 2064 (06.01) print resistance of lacquers, test, D 2091 (06.01) Impurities analysis of styrene by capillary gas chromatography, test, D 5135 (06.03) Impurities--paints/related coatings/materials analysis of major drgahic impurities in phenol produced by the cumene process, by gas chromatography, test, D4961 (06J03) analysis ofp-xylene, by gas chromatography, method, D 3798 (06,03) chemical analysis of benzene, by gas chromatography, test; ~ D 4492 (06.03) . _. impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) purity of propylene glycol monomethyl ether/dipropylene giycol monomethyi ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) pyridine base content in cresylic acid, by direct titration, test, D 4471 (06.03) styrene, by gas chromatography, test, D 3962 (06.03) Inclined plane method static friction of coating surfaces, test, D 4518 (06.01) Inclusions continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) Index of refraction (refractive index) See Refractive index Indian ocher See Ocher Indian red See Iron oxide red Industrial aromatic hydrocarbons See Hydrocarbons--industrial aromatic 1)59 DUP0502 98335 j _ ., Jndex ofASTM Standards, Section 6 Industrial grade benzene/toluene/xylene ' 'Vim Industrial grade benzene/toluene/xylene See Benzene/Toluene/Xylene (headings) Industrial materials/applications--chemicals Sa Chemicals establishing procedures to qualify/certify inspection for coating work in nuclear fatalities, * 04-&73|iKflV, inspection of linings in operating,flue gas systems, practice, D 4619 (06,01) solidification point of industrial organic chemicals, test, D 1493 (06.03) painting inspectors (metal substrates), gulch., i> 3.27/,1 * specifying inspection requirements forcoatmg/'muitd "l',i Industrial materials/applications--paints/related coatings metal substrates, guide, O 5I6| (OB.Ol) , ` rjJ|jK| testing industrial water-reducible coatings, guide, D4712 (06.0,1) Inspection personnel J^jpiil viscosity of paints/related materials, by ISO flow cups, test, establishing procedures to quaiify/eertifyinspect m-iaZ-soiii D 5125 (06.03) for coating work in nuclear facilities, guide, p 44Jjryg Inert pigments See Extender pigments Instrumental measurement--color/light See Light--exposure .. Infrared (IR) analysis qualitative identification of polymers in emulsion paints; by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) Instrumental measurement--paints/related cu uingsrnunbnaJ^Sfnl accelerated testing of paints/vamishes/laco ucrstieV d oroikioi*?*! using filtered open flame carbon-arcli.hi^aiircxposiitfi.i. apparatus, practice, D 822 (06.01) - ij.'-Hr * Infrared (IR) analysis--paints/related coatings/materials cellulose nitrate in alkyd lacquers, quantitative determination by infrared spectrophotometry, test, D3133 (06.01) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, 0 2621 (06.01) temperature of applied coatings on wood products during .the curing cycle, fry infrared radiation thermometers, practice, 0 3259(06.01) Infrared pyrometer temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, 0 3259 (061)1) Infrared spectrophotometry See Spectrophotometry--infrared Infusorial earth See Silica--diatomaceous Inhibitor zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Inhibitor content p-rerf-butyicatechol (TBC) in styrene monomer, test, 0 2120 (06.03) residual p-tert-butylcatechol (TBC) in styrene monomer, by addition cf .NaOH, test, D 4590 (06.03) , Ink apparent tack of printing inks/vehicies, by inkometer. test, 0 4361 (06.01) clarity/cleanness of (nonpigmented) paint ant} ink Hquids,.by visual examination, test, 0 2090 (06,02, 06.03) lightfastness of printed matter, D 3424 (06.01) nonvolatile content of printing inks/resin solutions/vehicfe, test. 0 4713 (06.01) water pickup oflithographic printing inks/vehicies in a laboratory mixer, test, D 4942 (06,01). Inkometer method apparent tack df printing inks/vehicies, by inkometer, test, 0 4361 (06.01) ' Inorganic colored pigments chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, 0 50, (06.02) bond strength of thermoplastic traffic marking niiterufls/ihibjjt^t cement bricks/steel cubes, test, D-4796 016.01).: ,-y Xi\ cathodic disbonding of pipeline coatings, accelerated prWanss'J test, G 8 (06.01) -y, 'S{ directional reflectance factor (45-deg 0-deg ' 1 optqoefif' * specimens, bv broad-band filter refleclome p lest' v'A. E 97 (06.01) evaluation of color for thermoplastic traffic Tnaikmg.maSrii " test, 04960 (06.01) S>W 5 gloss of higb-gloss metallic/nonmetallic si daces, by Scutiopti metry, method, E 430 (06.01) i relative tinting strength of white pigments, by rcfleet-iiWK-^. measurements, test, 02745 (06.02) , ' jj/SL testing industrial water-reducible coatings, guide! 047)1*(%<? Insulating coating systems cathodic disbonding of pipeline coatings, acu ie.ated pfoietiu test, G 8 (06.01) effects of outdoor weathering on pipeline mu ng', GII (06.01) specific bendabiiity of pipeline coatings, test, G II) (Op.U.IjA " water penetration into pipeline coatings, test, G 9 (06.<y,)" Interchemical wet film gage ii % wet film thickness of organic coatings, O 1212 <06.0lj|f Interior mold environments See Resistance--bacteria Interior paints/coatings efflorescence (of interior wall paints), test, D 1736 (g interior latex semigloss/gloss paints, selecting test guide, D 4540.(06.01) , * -,W"a latex flat wall paint, practice for selection and use nftest. procedures, p 2931 (06.01) practical washabiiity of orgapje epatihgs,' test, 0 4828 0Kfrrv scrub-to-failufe Of interior latex fiat wall paints,.test, * i.\. 0 2486(06.01) - solvent-thinned flat wali paint, practice for selection and ust'dl,'? test procedures, D3323 (06.01) ; Jh`?. solvent-thinned wall/trim semigloss enamels, praefre tor selection and use of test.procedures, D3425 (06.01) testing solvent-borne architectural (interior/exterior) guide, 05146(06.01) Inorganic linings inspection of linings in operating flue gas desulfurization systems, practice, 0 4619 (06,01) Insoluble matter content lead peroxideAnie red lead content ofdry red lead pigments, test, 0 49(06.02) sampling/testing lac resins (orange shellac/button tac/gamet lac/bleached lac), test, 0 29 (06.02) testing water resistance of coatings at 100 % relative hu practice, D 2247 (06.01) wet abrasion resistance of interior paints to scrubbing; by 1 loss, test, 0 4213 (06.01) Interlaboratory testing conducting interlaboratory study to determine precision oft method, practice, E691 (06.03) paints/related coatings, practice, 0 3980 (06.01) 1. f Inspection--coating applications Internal indicntor method design/fabrication offlue gas desulfurization system components (for protective lining application), spec., 0 4618 (06.01) acid number of rosin, test, D 465 (06.03) saponification number of rosin, test, D 464 (06.03) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, 05163(06.01) Internal voids -Ur continuity verification ofliquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) 1160 |acid| |saBf| ! sairf cH HB' HHSSs s DUP050298336 Index of ASTM Standards, Section 6 Isopropylbenzene (cumene) Intrinsic viscosity ' Sa Viscosity (headings) intrinsic viscosity of cellulose acetate, using modified Baker-Philippoffequation, test, D 871 (06.02) limiting viscosity number of cellulose acetate propionate/ butyrate, test, A D817 (06.02) odine-pyridine-sulfur dioxide reagent water in liquid naval stores, test, D 890 (06.03) Iodine reagent merited water content, in phenol and related materials, test, D 1631 (06.03) (Iodine value acid/amine value of fatty quaternary ammonium chlorides, test, | D 2078 (06,03) , [' fatty amines, amidoamines, and diamines, Wijs procedure, test, D 2075 (06.03) I; sampling and testing shellac varnish, D 1650 (06.02) I sampling/testing lac resins (orange, shellac/button lac/gamet { lac/bleached lac), test, t> 29 (06.02) Iodine value--drying oils and their derivatives modified RosCnmund-Kuhnhenn method, test, 0 1541 (06.03) Wijs method, test, D 1959 (06.03) Ionic contamination See Contamination (headings) Iron raw/bumt sienha pigmentsj spec., D 765 (06.02) : Iron blue '1 chemical analysis of (irdn/copper phthalbcy&iiihe/ultramarine) blue pigments, test, D1135 (06.02) chemical analysis of phthalocyahine blue/green pigments, test, D32S6 (06.02) iron biuepigment, spec., 0261 (06.02) Iron content--paint driers formaldehyde, test, D 2087 (06.03) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test, D 2363 (06.02) iron in liquid iron paint driers, by EDTA method, test, D 3804 (06.03) iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) methylcellulose, test, D1347 (06.02) rosin, test, D1Q64 (06.03) Iron oxide black black synthetic iron oxide pigment, spec., D 769 (06,02) iron oxide black (natural)- chemical analysis, test, , D 3872 (06.02) Iron oxide brown (natural) ' analysis, D 50 (06.02) ; natural red/brown iron oxide pigments, spec., D 3722 (06.02) Iron oxide brown (synthetic) iron oxide black (natural)- chemical analysis, test,. D 3872 (06.02) synthetic brown iron oxide pigment, spec., D 3724 (06.02) Iron oxide content calcium borosilicate, test, D 4487 (06.02) Iron oxide red (natural) analysis, D 50 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) Iron oxide red (synthetic) analysis, D 50 (06.02) synthetic red iron oxide pigment, spec., D 3721 (06.02) Iron oxide yellow analysis, D 50 (06.02) yellow iron oxide (hydrated), spec., D 768 (06.02) Iron paint driers See Driers Irradiance/irradiation--paints/related coatings/materials effects of radiation on coatings (for light-water nuclear power plants), test, D 4082 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Isatin thiophene content of benzene, by spectrophotometry, test, D1685 (06.03) Isobutanol See Isobatyl alcohol Isobutene (isobutylene) purity of hydrocarbons from freezing points, test, D1016 (06.03) Isobutyl acetate alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) isobutyl acetate (95 % grade), spec., D 1718 (06.03) Isobutyl alcohol isobutyl alcohol, spec., D1719 (06.03) isocyanate group content of urethane materials/prepolymers, test, D 2572 (06.02), ISO cups viscosity of paints/related materials, by ISO flow cups, test, D 5125 (06.03) Isocyanates isocyanate group content of urethane materials/prepolymers, test, D 2572 (06.02) ISO (Internationa) Standards Organization) index of standards by ISO/TG 35 on Paint and Varnishes, (Related Material) (06.01,06.02, 06.03) Isomer analysis xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) Isooctane purity of hydrocarbons from freezing points, test, D1016 (06.03) Isophorone isophorone, spec., D 2916 (06.03) Isophthalic acid content isophthalic acid content of alkyd/polyester resins, test, D 2690 (06.02) Isoprene purity of hydrocarbons from freezing points, test, 0 1016(06.03) Isopropanol . ._ flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) Isopropyl acetate alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) , isopropyl acetate (99 % grade), spec., D 3131 (06.03) Isopropyl alcohol isopropyl alcohol, spec., D 770 (06.03) Isopropylbenzene (cumene) Sa Cumene (isopropylbenzene) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) benzene content of cyclic hydrocarbon products, by gas chromatography, test, 0 4534 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) isopropylbenzene (cumene), spec., D 4077 (06.03) phenol content of (refined) isopropylbenzene (cumene), test, ' D 3160 (06.03) purity analysis of isopropylbenzene (cumene), by gas chromatography, test, D 3760 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, 0 3437 (06.03) 1161 DUP050298337 Index of ASTM Standards, Section 6 4,4' Isopropylidene diphenol 4,4' Isopropylidene diphenol sampling/handliag 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) solidification point, test, D 4493 (06:03) solution color of 4,4'-isopropylidenediphenoI (dissolved in methanol), test, D 4789 (06.03) Ivory black See Bone black Jaune de zinc See Zinc yellow " Joints comparative corrosion preventive characteristics Of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) ' j Jones reductor total titanium in white titanium pigments, by Jones reductor, test, D1394 (06.02) K Kaolinite See Aluminum silicate pigments \ Karl Fischer reagent method--water content , paints/paint materials, test, 04017 (06.01) water in volatile solvents, by Fischer reagent titration method* test, D1364 (06.03) Kauri-butanol value * hydrocarbon solvents, D 1133 (06.03) Ketones aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) , , ,, MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent mb, test, D 4752 (06.01) , methyl ethyl ketone, spec., D 740 (Q,6.Q3) methyl isoamyl ketone, spec., 0 2917 (06.03) ., methyl isobutyl ketone, spec., 0 1153 (06.03) methyl -amyi ketone (98 % grade), spec., 0 4360 (06.03) purity of aldehydes and ketones, test, 0 2192 (06103) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, 0 3893 (06.03) purity of methyl ethyl ketone, using gas chromatography, test, 0 2804(06.03) purity of methyl isobutyl ketorte, by gas chromatography, test, 0 3329(06.03) Kiln-dry bleached lac See Bleached lac Kiln pine tars ` See Oils--pine (natural/synthetic) Knife test ' adhesion of coating films to metallic substrates, by tapetest, 0 3359 (0601) Knuop hardness indentation hardness of organic coatings, by Knoop and Pfund methods, test, 0 1474 (06.01) Konig pendulum test hardness of organic coatings, by Konig/Persoz pendulum hardness tests, D 4366 (06.01) Kreras white See Basic carbonate white lead Kubelka-Munk equation relative tinting strength of printing ink dispersions, test, 0 2066(06.01) Labeling abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, 05181 (06.01) art materials for chronic health hazards, Drac.-iiv D 4236 (06.01) , ,,, , Laboratory ''> rt evaluating arid comparing tratoifef condliioi.s-lei-Mr'.f,,;'^ conditions, test, 0 5009 (06.01) ' > profile of abrasive blast-cleaned steel wrl,ices 11 laborator Mw field/fabricatiug shop, test, 04417 (Ob.OlJ * " . V, Laboratory mixer ' - waterlapbiocrkautporoyfmlitihxoegr,ratepsht,icDp4r9in4t2ing(06in:k0s1/)ve. hicl.js tn u J ' LAC orange shellac and (button lac/gamet lac), spc,. 0 '37 (06104 Mlt'? Lacquer ' >' : . * abrasion resistance^ by air blast abrasion test 0l>'S (lie. Ill paint/vamish/lacquer/i-elated products) leu 01613 (06.03) ! - " ' > Ai/'jii; HIadhesion (to smooth surfaces), by scrape adhesion test. : D 2197. (06.01) ? .' '-Vi amount of liquid separated as upper layer from a \i> " '' solution/dispersion containing dispersed *ohds, fc-t D4948 (06.01) 1r cellulose nitrate in alkyd lacquers, quantitative detcimmat'uifi infrared spectrophotometry, test,,0 313,3 (1)6.01) . "v ' clarity/cleanness Of (nonpigmented) paint and 111k liquuL,hy.' ,,yisual,e*ainingtiqn,,tet, D 2090 (06.02, 06.03) . ,*TU " clear and pigmented, selection oftest!methods, O 333 ' J ** clear/pigmeotod organic costings, (0^,0,1318 (06 01) conducting tests oh paint/varhish/Iacquer/relatul prod using enclosed carbon-arc light/water exposure jp practice, D 5031 (06.01) discoloration (light stability), test, D 2620 (06 01) * ' ' p, dry film thickness of noncondttetive'coatings (anpli^ to t noriferfOus ltietaLb'ase), tiohSdestrtictive'int.im 11 111 e . D1400 (06.D1) '' dry film thickness ferrous base), (of nonmagnetic 01186 (06.01) Ofgkriic'co.itiriys apKpliedWm dry-film thickness of organic coatings, uring microiutte.s, Ust, 1 i D1005 (06.01) effects Of overbaking on'organic coUtfrigs, practice, D 2454 (06.01) ' ' ,3*J^ 'A? elongation/tensile strength/stiffness,, test, 0 2370 (06.01) , ester value of solvents and thinners, lest.'D 1617 (06.03) `4 field identification of coatings, test, 0 5043 (06.01) * film formation rates in drying or curing process, at foiarfr'<l j* temperature, test, D 1640 (06.01) ' flash point of`liquids," by'SetaflaSti closed-cup apparatus, tedtpw 03278(06.03) freeze-thaw stability of multicolor lacquers, test, 0 2337 . glacial acrylic acid (99.0 % grade), spec., 0`4416 (06.03) . "S heptane miSnbility of lacquer.solvents, test, 01476;(O6.03), * imprint resistance, of dried films, test, 0 2091 (06.01) -tnt indentation hardness oforganic coatings; by Knoop and Pfund ; methods, test, 0 1474 (06.01) <' methyl n-amyi ketone? (98 % grade),-spec., 04360 (06.03) moisture vapor transmission of organic coating films, test, 0 1653 (06.01) paint/varnish/lacquer/related products, terminology, : D 16 (06.01, 06.02, 06.03) ' paint/vamish/iacquej/related. products, test, A 0 1475 (06.01)' particle size analysis (of multicotored/nitrocellulose-base ' s lacquer), test, A 0 2338 (06.01) ' \ plasticizer migration from vinyl fabrics to lacquers, method, " * D 2199 (06.01) ' ` preparation of free films of organic coatings, practice, '' _i " 0 4708(06.01) preparing glass panels for testing; 0 3891 (06.01) 1 resistance to failure (on steel sur&ces), by water immersion test, * 0 870(06.01) 1162 DUP050298338 r Index of ASTM Standards, Section 6 stain removal (of multicolored lacquer on primed steel panels), _ test, D 2198 (06,01) gj, standard environments for conditioning/testing paint/ varnish/lacquer/related materials, spec., D 3924 (06.01)- jj:. temperature-change (high-low) resistance of clear, nitrpcellulose lacquer films applied to wood, test, J) 1211 (06.01) viscosity of paints/varnisbes/lacquers, by Ford viscosity cup, test, D1200 (06.01) " Viscosity (of paints/varnishes/lacquers/rClated materials), by dip-type viscosity cups, test, D 4212 (06.01)- ' wet film thickness of organic coatings, D 1212 (06.01) wet film thickness of organic coatings, by notched gages, ' practice, D4414 (06.01) wood furniture lacquers, test, D 2571 (06.01) |Lac resins . See Resins--lac , ELampblack [r lampblack pigment, spec., D 209 (06.02) solvent extractable material in black pigfnents, test, || D 305 (06.02) ILampblack content '' " solvent extractable material in'black pigments, test, ' D 305 (06.02) gLapis lazuli ft See Ultramarine blue .. gtatex paints antimony cqntent (low concentrations) in solids of liquid ; : coatings/dried films, by atomic absorption spectroscopy, - test, D 3717 ^06.01) . , - ", artiste' abrylic emulsion paints; spec., D 5098 (06.01) blocking resistance of trade sales paints, test, i> 4946 (06.01) chromium content (low concentrations) Mr Solids of liquid ' t- coatings/dried films, by atomic absorption spectroscopy, test, D 3718 (06.01) , coarse particles in pigments/pastes/paints, test, D 185 (06.01, 06.02) color differences of opaque materials, instrumental evaluation, test, D 2244 (06.01) comparison of the brush1 drag of latex paints, test, D 4958 (06.01) conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) consistency of paints, using Stormer viscometer, test, . , D 562 (06.01). directional reflectance factor (45-deg O-deg) of opaque specimens, toy broad-band filter reflectometry, test, .E97 (06.01) drying/curing/film formation (at room temperature), test, D1640 (06.01) efflorescence (of interior wall paints), test, 0 1736 (06.01) field identification of coatings, test, D 5043 (06.01) filter-retained solids content.of polymer latexes, test, D 5097 (06.02) fineness of dispersion of pigment-vehicle systems, test, D1210 (06.01) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) gloss/sheen uniformity evaluation, test, D 3928 (06.01) hiding power of architectural paints applied by roller, test, D 5150 (06.01) hiding power of paints, by reflectometry, test, A to 2805 (06.01) hiding power (relative dry), visual evaluation of brushouts, test, D 344 (06.01) ' high shear viscosity (of paints/varnishes/related products), by 1CI cone/plate viscometer, test, D 4287 (06.01) " lead/cadmium/cobait content (low concentrations) in - nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) leveling, by draw-down method, test, to 4062 (06.01) low temperature coalescence, test, to 3793 (06.01) Lead chromate mandrel-bend test of attached organic cbatings, test, D522 (064)1) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, to 3624 (06.01) nonvolatile content of latexes, test, D 4758 (06.02) package stability of solvent-reducible/water-reducible paint, test, D1849 (06.01) paint spatter resistance to roller application, test, to 4707 (06.01) paint/varnish/lacquer/related products, test, A to 1475 (06.01) preparing drawdowns of artists* paste paints, practice, D 4941 (06.01) producing films ofUniform thickness of paiat/vatnish/related products on test panels, test, t> 823 (06.01) qualitative identification of polymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D3168 (06.01) relative tinting strength of chromatic painty test, D 4838 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D1848 (06.01) sag resistance, using multinotch applicator, test, to 4400 (06.01) sampling liquid paints/related pigmented coatings, practice, D 3925 (06.01) scrub-to-failure of interior latex flat wall paints, test, 2486 (06.01) specular gloss of nonmetallic specimens, test, D 523 (06.01) testing water resistance* of coatings at 100 % relative humidity, practice, D 2247 (06.01) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) volatile content, test, D 2369 (06.01) volatile organic content (yOC) of isaints/related, coatings, selecting test procedures, practice, D 3960 (06.01) volume nonvolatile matter in clear/pjgmented coatings, test, D 2697 (06.01) washability of interior architectural coatings, test, D 3450 (06.01) water content of paints/paint materials, by Karl Fischer method, test, O 4017 (06.01) water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) , water-thinried floor paints, selection and use of test procedures, practice, D 3358 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D42t3 (06.01) . wet-to-dry hiding change of architectural coatings, test, 0 5007(06.01) wood used as panels in weathering tests of coalings, spec., 1)358(064)1) Latex paints--selection and use of test procedures exterior latex house paint, practice, D 3129 (06.01) floor paint, practice, D 3358 (06.01) interior flat wall paint, practice, D 2931 (06.01) interior latex semigloss/gloss paints, selecting test methods, guide, D 4540 (06.01) latex vehicles, selecting test procedures, practice, D 4143 (06.02) Latex vehicles nonvolatile content of latexes, test, D 4758 (06.02) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) Leachates/leaching water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) Lead chromate chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) 1163 DUP050298339 Index of ASTM Standards, Section 6 Lead chromate lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (06.02) Lead chromate pigment yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) operating light-/water-exposure apparatus (fluoresccnt-LV coiidensation type) for exposure of nonmetallic materials practice, G 53 (06.01) Lead content--paints/related coatings/materials analysis of white zinc pigments, test, D 3280 (06.02) chromium' trioxide content of basic lead silico-chromate pigment, test, D1844 (06.02) detection of lead in paint/dried paint films, test, D3618 (06.01) lead/cadmium/cobalt content (low concentrations) in nonvolatile portion ofliquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D4358 (06.02) lead content in paint, by direct aspiration atomic absorption spectroscopy, test, D 4834 (06.01) lead peroxide/true red lead content of dry red lead pigments, test, B' 49 (06.02) liquid paint driers, selection of test methods, D 564 (06.03) paint driers, by EDTA .method, test, D 2374 (06.03) white linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (06.01) yellow/orange/green pigments containing lead chromate/ chromium oxide green, test, D126 (06.02) Leaded zinc oxide analysis of white zinc pigments, test, D 3280 (06.02) Lead peroxide content lead peroxide/true red lead content of dry red lead pigments, test, D49 (06.02) Lead salt infrared radiation thermometers i temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, 03259(06.01) Lead screening test lead content in paint, by direct aspiration atomic absorption spectroscopy, test, D 4834 (06,01) Lead silicochromate lead/qhromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (06.02) Leafing properties sampling/testing flaked aluminum powders/pastes, methods, D48tf (06.03) Leveling characteristics architectural paints/coatings (aqueous/nonaqueous), in white/light tints, by draw-down method, test, D 4062 (06,01) Lieberman-Storch test qualitative detection of rosin in varnishes, by LiebermanStorch/Halphen-Hicks tests, D 1542 (06.01, 06.02) Light--exposure accelerated testing of.paints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D 822 (06.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) cure time of ultraviolet-cured coatings, practice, D3732 (06.01) exposure of paints/related coatings to fluorescent UVcondensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) lightfastness of pigments (in artists' paints), test, D 4303 (06111) lightfastness of printed matter, D3424 (06.01) operating carbon-arc light-exposure apparatus with and without water for exposure of nonmetallic materials, practice, G 23 (06.01) Light--lightfastness lightfestuess of pigments (in artists' paints), test, D 4303 (06.01) printed matter, D 3424 (06.01) Light--reflectance See Reflectance and reflectivity (headings) Light--stability clear coatings, by sunlight-through-glass method, test, D 2620 (06.01) Light--transmission and reflection color changes (of opaque materials), by instrumental etaljation test, D 2244 (06.01) gloss differences between surfaces of similar appearance, method for visual evaluation, D4449 (06.01) light stability of clear coatings, by sunlight-through-glass method, test, D 2(120 (06.01) Lightening power See Tinting strength Lightfastness artists'acrylic emulsion paints, spec., D 5098 (06.01) Limestone drop test impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) .; ; Limiting viscosity number limiting viscosity number of cellulose acetate, propionate/ butyrate, test, A D 817 (06.02) Limonite See Ocher Linear programmed temperature gas chromatography See Chromatography--gas (headings) Lining industry continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) design/use of safety alert system for hazardous work locations in coating/lining industry, practice, A D 4257 (06.01) inspection of linings in operating flue gas desulfurization ~ systems, practice, D 4619 (06.01) Linings continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06,01) protective coating/iining work for power generation facilities, terminology, D 4538 (06.01) specifying inspection requirements for coating/lining work on metal substrates, guide, D 5161 (06.01) Linings--defects and failures photographic documentation of coatings/lining defects and failures, D 4121 (06.01) Linseed oil absorption (by pigments), by Gardner-Coleman method, test, D 1483 (06.02) absorption (by pigments), spatula rub-out test, D 281 (06.02) boiled linseed oil, spec., O 260 (06.03) linseed oil, spec., D 1538 (06.03) raw, foots, by gravimetric method, test, D 1966 (061)3) , raw, foots, by volumetric method, test, D 1954 (06.03) raw linseed oil, spec,, D 234 (06.03) white linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (06.01) 1164 iipids alcol . Liquid < Liquid !; test Liquk !! sail | Liquk | Liquk ! p ( jLiqui am chj cla Loa if- (Is i f DUPO 50298 340 Index of ASTM Standards, Section 6 |jipids 1 alcohol-benzene soluble matter in cellulose, test, D 1794 (06.02) liquid chemicals See Chemicals liquid coating properties I' testing solvent-borne architectural (interior/exterior) coatings, guide, D 5146 (06.01) quid cyclic products sampling/handling liquid cyclic products (at ambient temperature), practice, 03437 (06.03) liquid driers See Driers liquid epoxy resins Sa Resins--epoxy epoxy content of epoxy resins, test, D 1652 (06.02) aquids amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) chemical resistance of pipeline coatings, test, G 20 (06,01) clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02,06.03) color of transparent liquids, by Gardner color scale, test, 01544 (06.01,06.02, 06.03) commercial density (of pure liquid chemicals), test, D 3505 (06.03; flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) flash point by Tag closed tester, test, D 56 (06.03) flash point (of fuel oils/iube oiis/suspension of solids/Iiquids), by Pensky-Martens closed tester, test, 0 93 (06.03) liquid/solid status (of viscous materials), test, 1)4359 (06.01) oiticia oil (permanently liquid), spec., D 601 (06.03) sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, D 4206 (06.01, 06.03) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) viscosity of transparent liquids, by bubble time method, lest, D1545 (06.01, 06.02; 06.03) f Lithium methoxide . identification of carboxylic acids in alkyd resins D 2455 (06.02) |liOading tests puli-offstrength of coatings, using portable adhesion testers, test, 04541 (06.01) |Loading tests--metals/alloys : salt spray (fog) testing, method, B117 (06.01) iLoss of adhesion See Adhesion--loss of adhesion |Toss of coolant accident (LOCA) conditions See Nuclear reactor vessels--light-water cooled |Loss on ignition See Ignition--loss on ignition | Low concentrations (of elements) antimony content (low concentrations) in soiids ofliquid coatings/dried films, by atomic absorption spectroscopy, test, 03717 (06.01) chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3718 (06.01) lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3335 (06.01) mercury content (low concentrations) in liquid coatings/coatings vehicles/dried films, by atomic absorption spectroscopy, test, D 3624 (06.01) j Low hiding strontium chromate See Strontium chromate I Low temperature bake coatings nonvolatile content of latexes, test, D 4758 (06,02) Marine (shipboard) coatings Low voltage wet sponge test discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D5162 (06.01) Luminous reflectance See Reflectance and reflectivity (headings) M Magazine covers abrasion resistance of printed matter, by the ga-cat Comprehen sive abrasion test, D 5181 (06.01) Magnesium alloys surface preparation for painting, practice, D1732 (06.01) Magnesium anode method cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) Magnesium carbonate acid-insoluble extenders in (iron/copper phthalqcyanine) ultramarine) blue pigments, test, D 1135 (06.02) Magnesium oxide (MgO) content magnesium oxide in magnesium silicate pigment, test, D 717 (06.02) Magnesium silicate magnesium silicate pigment (talc), spec., D 605 (06.02) Magnesium sflicate.pigment magnesium silicate pigment, analysis, test, D 717 (06.02) Magnetic flux film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Magnetic testing film thickness of pipeline coatings on steel, nondestructive measurement, method,,G12 (06.01) Maintenance--coatings assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) conducting a patch test to assess coating compatibility, practice; D 5064 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, D 5163 (06.01) Maleic add content maleic acid content of maleic anhydride, by potentiometric titration, test, D 2930 (06.03) Maleic anhydride color in molten state/after heating, by platinum cobalt scale . (includes phihalic anhydride), test, D 3366 (06.03) maleic acid content of maleic anhydride, by potentiometric titration, test, D 2930 (06>03) maleic anhydride, spec., D 3504 (06.03) sampling and handling aniline, practice, D 3438 (06.03) Mandrel bend test mandrel bend test of attached organic coatings, test, D 522 (06.01) Manganese black synthetic iron oxide pigment, spec., D 769 (06.02) liquid paint driers, selection of test methods, 0 564 (06.03) " raw/burnt sienna pigments, spec., O 765 (06.02) synthetic red iron oxide pigment, spec., D3721 (06.02) Manganese content metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) paint driers, by EDTA method, test, D 2375 (06.03) Manufacturing processes transfer efficiency under production conditions for spray application of automotive paints, by weight basis, practice, D 5066 (06.01) Marine (shipboard) coatings See Antifouling paint pigments (headings) 1165 DUPO 50298341 Index of ASTM Standards, Section 6 Mar resistance Mar resistance mar resistance of organic coatings, using balanced beam scrape adhesion and mar test, D 5178 (06.01) Masonry assemblages making and preparing concrete/masonry panels for testing paint finishes, method, D 1734 (06.01) surface cleaning concrete unit masonry (for coating), practice, D 4261 (06.01) Masonry water repellents nonvolatile content in silanes/siloxanes/siiane-siloxane blends used in masonry water-repellent treatments, test, DS095J06.01) Material handling impact resistance of pipeline coatings, by falling weight test, G 14 (06.01) naphthalene, maieic/phthalic anhydride, practice, D 3438 (06.03) phenol-and cresyiic acid, practice, D 3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) Matter insoluble in chloroform chloroform insoluble matter in oiticia oil, test, D 1958 (06.03) Mechanical damage specific bendability of pipeline coatings, test, G 10 (06.01) Mechanical muller See Muller device MEHQ content See Methyl ether of hydroquinone (MEHQ) content MEK (methyl ethyl ketone) resistance See Methyl ethyl ketone (MEK) Menhaden-derived fish oil See Oils--drying ' Mereaptans mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06.03) Mercuric oxide analysis, D 284 (06.02) mercuric oxide for use in antifouling paints, .spec., 1)911 (06.02) Mercury content dry mercuric, oxide pigment, test, D 284 (06.02) mercury content (low concentrations) in liquid coatings/coatings velTicles/dried films, by atomic absorption spectroscopy, test, D 3824 (06.01) Mesityl oxide analysis of major organic impurities in pheilol produced by the cumene process, by gas chromatography, test, D4961 (06.03) , Metallic copper content chemical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) Metallic finishes gloss of high-gloss metailic/'nonmetallic surfaces, by goniophotometry, method, E 430 (06,01) Metal powder pigments See Aluminum powder and paste/Copper powder Sa Gold bronze powder/Zinc dust Metal primer Sa Primer zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Metals and metallic materials wet film thickness of organic coatings, D 1212 (06.01) Metals and metallic materials--coating applications accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D4141 (06.01) adhesion of coating films to metallic mbit9 G -, hv 1i D 3359 (06.01) * coil coatings, testing, practice, D 3794 (06.01) discontinuity (holiday) testing of nnniondiiLtne i coating on metallic substrates, pruui,,e, D-Sj,62 flexibility/adhesion of organic coatings (paint .j on. jxepam deformed metallic sheets, test, D 4145 (06 01 j '-11 t,u r gloss of high-gloss metaUic/nonmetallio tiu|lUi hv* untcmhrrfit` metry, method, E 430 (06.01) I mandrel bend test of attached organic toatups. test "1 D 522 (06.01) ' metals (iron/copper/manganese/calcit m) cot ten oi_ pulp (from wood/cotton), by atomic spccircnhotom"" test, D 4085 (06.02) * painted surfaces- evaluating degree of blistering AD 714 (06.01) specifying inspection requirements foi c uting linmd metal substrates, guide, D 5161 (06.01) j> testing primers/primer surfacers over preformed mejiil* 't selection/use of procedures, prac ic,, D 1322'(llfc'fil)K`)^tSt Metaxylene .. See mela-Xylene Methacrylic add (glacial) . ``-ti glacial (98,5 %) methacrylic add (for twj m iwiom Jtl lacquer/reiated products), spec., D 3845 (06 03) * `-to. |r Methanol (methyl alcohol) ** < Sa Chemicals/Petroleum and pi trolium products $ iij (headings) ; tllj '|f acetone in methanol (methyl alcohol) let, D 16l.2,(06l&)^ methanol content of formaldehyde soluti in D 2380 (06.0) 1111 methanol (methyl atcdhol), spec., D1152 (1)6 03) permanganate tiifie of acetbne/mefhanol, tes D ,1 solution color of 4,4'-isopropyiidenediplitMial (cte methanol), test, D 4789: (06.03) Methoxy ethanol 2-methoxyethanoi, spec., D 3128 (06.03) Methoxyl content v hydrogen sulfide/sulfur dioxide (qualit't,ivei of in aromatic hydrocarbons, test, D 2163 (06.02) , methylceliulose, test, D1347 (06.02) Methoxyl/hydroxypropy! substitution s cellulose ether products, by Zdsel-gas chronuiojreph D 3876 (06.02) ' Methyl acrylate methyl acrylate, spec., D 4709 (06.03) Methyl amyl acetate methyl amyl acetate, spec., D 2634 (06 03) Methyl amyl alcohol See Methyl isobutyl carblnol Methyl amyl ketone (MAK) methyl n-amyl ketone (98 % grade), spec., I) 4360 {0 purity of methyl (amyl ketone/isoam; I ketone), by gas d,,--, chromatography, test, D 3893 (06.03) *n) (' ^ Methylbenzofuran analysis of'major organic impurities in i nen'l pfnJuf cumene process, by gas chromatography, test,1 D 4961 (06.03) Methyl butyl ketone purity of methyl (amyl ketone/isoamyl ketone), bygas"4 chromatography, test, D 3893 (06 U11 1 Methylceliulose See Cellulose and cellulose derb.itiw.'. * *l Methylcyclohexane purity of hydrocarbons from freezing points, test, ' D 1016 (06.03) Methylene chloride dichloromethane/l,l,l-trichloroethanc umlci t in pi ms/ coatings, by direct injection gas i Ilium noguiphy1, lest. D 4457(061)1) 1166 DUP050298342 Index of ASTM Standards, Seuidn 6 Mo'^iun eiii'ifciit -paints/rc I.iteil coatings/materials Methyl esters Microscopic examination-- paiots/rduied coatings fatty add composition, by gas-liquid chromatography of methyl di\ film thickness oi pru'cctne on rang systems, by destructive esters, test, D1983 (06.03) means, test, D 4138 (06.01) j preparation from oils, for fatty acid composition determination repoi iinij particle sin. iiiuijeiuu.ucc of raiments, practice, j by gas-liquid chromatography, D 2800 (06.03) 0 1366 (06.02) f preparation of methyl esters from fatty acids, for fatty add Microwave procedures !, composition analysis, test, D 3457 (06.03) laboratory preparation of gelled vehicles) using-microwave oven, Methyl ether of hydroquinone (MEHQ) content practise. D 5166 (06.02) 1 methyl ether of hydroquinone (MEHQ) content of colorless Migration monomeric acrylate esters, test, 0 3125 (06.03) plasticizer migration from vinyl fabrics to lacquers, method, Methyl ethyl ketone (MEK) ; MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent; rub, test, D 4752 (06.01) methyl ethyl ketone, spec., D 740 (06.03) D 2X99 (06.01) Milliequivalency acid/base miUiequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) purity of methyl ethyl ketone, using gas chromatography, test, Milori blue 0 2804(06.03) See Iron blue Methyl isoamyl ketone (MIAK) methyl isoamyl ketone, spec., D 2917 (06.03) Minerals field identification of coatings, test, D 5043 (06.01) purity of methyl (amyl ketone/isoamyl ketone), by gas Mineral spirits chromatography, test, 0 3893 (06.03) aromatics (ethylbenzene and eight-carbon (Cs/heavier) content Methyl isobutyi; carbinoi methyl isobutyl carbinoi, spec., O 2635 (06.03) Methyl isobutyi ketone (MIBK) methyl isobutyi ketone, spec., 01153 (06.03) purity of methyl isobutyi ketone, by gas chromatography, test, 03329 (06.03) Methyl methacrylate unreacted monomer content of latexes, by gas-liquid chromatography, test, 0 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, 0 4827 (06.02) Methylol group content methylol group determination (qualitative) in phenolic resins, test, 0 4706(06.02) Methylstyrene 1 analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test, 04961 (06.03) Metric practice--SI (International System of Units) use of international'system of units (SI) (modernized metric system), excerpts, (Related Material--all volumes) (06.01, 06.02,06.03) Mica pigment grit content of mica pigment, test, 0 716 (06.02) wet ground mica pigments, spec., 0 607 (06.02) Microbiological attack--paints/related coatings discoloration susceptibility (in exterior exposure tests), practice, 0 3456(06.01) paint films, evaluating degree of surface disfigurement, AD 3274 (06.01) resistance of emulsion paints (in containers) to attack by microorganisms, test, D 2574 (06.01) resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, 0 3273 (06.01) Microbiological examination presence of and removing microbial (fungal/algal) growth on paint/related coatings, guide, D 4610 (06.01) Microcoulometry See Coulometry--microcoulometry in mineral spirits, by gas Chromatography, test, D 3257 (06.03) mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235 (06103) porosity of paint films (to indicate coating penetration), test, 03258(06.01) Miniature sandmiil method color and strength of color pigments, A D 3022 (06.02) Minimum film formation (of paints) See Film--formation rates Minimum film formation temperature (MFFT) minimum film formation temperature (MFFT) of emulsion vehicles, test, D 2354 (06.02) Miscibility heptane miscibility of lacquer solvents, test, D 1476 (06.03) water miscibility of water-soluble solvents, test, D1722 (06.03) Mixed aniline point sampling and testing dipentene, method, D 801 (06.03) Mixed xylene See Xylene (mixed) MMFT See Film Model 'C' wet film thickness gage wet film thickness of organic coatings, D 1212 (06.0!) Modified Wolfe-potentiometric method See Wolfe-potentiometric method Moisture analysis--wood products edge performance of composite wood products under surfactant accelerated moisture stress, test, D 2Q65 (06.01) Moisture content--paints/related coatings/materials calcium borosilicate, test, D 4487 (06,02) capillary moisture in concrete, by plastic sheet method, test, D 4263 (06.01) cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, 0 871 (06.02) ethylceliulose, test, D 914 (06X12) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, tesl, D 2363 (06.02) hydroxyethylcellulose, test, D 2364 (06.02) hygroscopic moisture (and other matter volatile under test Microelectronic device processing--water conditions) in pigments, test, D 280 (06.02) reagent water, spec., D 1193 (06.03) methylcellulose, test, D 1347 (06.02) Micrometer moisture content of (iron/copper phthalocyanine/ultramarine) * disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) blue pigments, by Brabender test, D 1135 (06.02) moisture in cellulose, test, 0 1348 (06.02) dry-film thickness of organic coatings, using micrometers, test, pentaerythritol (for manufacture of alkyd/other synthetic resins), Si-5 'J "S 0 1005 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) tests, D 2195 (06.03) pine tars and pine tar oils, test, D 856 (06.03) sampling and testing dipentene, method, 0 801 (06.03) t 1167 DUP050298343 Index of. ASTM Standards, Section 6 Moisture content--paints/reiated coatings/materials sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, D 1439 (06.02) tall oil, methods of testing, D 803 (06413) water content of paints/paint materials, by Karl Fischer method, test, D4017 (06411). water in liquid naval stores, test, 0 890 (06.03) Moisture degradation conducting tests on paint/vamish/Iacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D5031 (06.01) Moisture passage ,, . water penetration into pipeline coatings, test, G 9 (06.01) Moistnre vapor permeability moisture vapor transmission of organic coating films, test, D1653 (06,01) Molar substitution (MS) hydroxyethylcellulose, test, D 2364 (06.02) Molecular weight--average acid/amihe value of fatty quaternary ammonium chlorides, test, D 2080 (06.03) Molybdate pigment molybdate orange pigments, spec., 0 2218 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Molybdenum content i molybdate orange pigments, spec., D 2218 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, 0 126 (06.02) Monocyclic aromatic hydrocarbons See Hydrocarbons (headings) , Monocyclic terpene hydrocarbons. See Dipeotene (and related terpene solvents) (headings) Monomeric acrylate esters (colorless) . methyl ether of hydroquinone (MEHQ) content of colorless monomeric acrylate esters, test, D 3125 (06.03) Monomers unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) water content of paints/paint materials, by Karl Fischer method, test, D 4017 (06.01) Monomer (unreactcd) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) Monopentaerythritol content monopentaerythritol in commercial pentaerythritol, by gas chromotography/dibenzal methods, test, D 2195 (06.03) Mortar resistance acid/mortaf resistance of factory-applied'clear coatings on extruded aluminum products, test, D 3260 (06.01) Mottling pressure mottling/blockmg resistance of organic coatings (on metal substrates), test, D 3003 (06.01) reporting paint film failures characteristic of exterior latex paints, classification, D 1848 (06.01) Mud-cracking reporting paint film failures characteristic of exterior latex paints, classification, 0 1848 (06.01) Muffle furnace nonvolatile and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (06.01) Muffle-furnace technique chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test,,D4797 (06,01) Muller device color/timing strength (of dry colored pigments/pastes in oil), test, D 387 (06.02) Multinotch applicator sag resistance of paints, using a multiuorrh <* D 4400 (06.01) p wet film thickness of organic coatings b- n.TM+, practice, 4414 (064)1) - Multipanel forms recording results on single-/tjfulti-pancl forms A D 1150 (06.01) N Naphtha and naphtha derivatives ,'J acidity of benzene/toluene/xylenes/solve u napl industrial aromatic hydrocarbons, test, D 8 add wash color of industrial aromatic hvdro D 848 (06.03) aromatic hydrocarbons/related chemicals, tsrmi D 4790 (06.03) "r'r.M't evaporation residue determination, test, 0 2232 high-flash aromatic naphthas, spec., D 3734 i06Jll) sampling and handling aniline, practice, D 3438 (06 03 ; \, '* VM & P naphthas, spec., D 3735 (06.03) A-] water content, by iodine reagentmethod, test, I) l63t^flfri Natural drying oils : ij. See Oils--drying v Natural iron oxide pigments See Iron oxide black . ' t, Natural pigments . J " '6' TV iron oxide black(natural)- chemical analysis, test D 3872 (06.02) natural red/brown iron oxide pigments, spec., D3722^t pure para red toner pigment, spec., 0 475 (06.02) 1 pure toluidine red toner, spec., D 656 (06,02) '"s;vSW Natural pine oil See Oils--pine (nalural/synthetic) Natural yellow oxide See Ocher, , Naval stores naval stores/reiated products, def. of terms, 0*804 (06 o' volatile/nonvoiatile content (ofdriers/drying oils/naval and solvents), selecting test procedures, guide, 04140(06.03) water in liquid naval stores, test, 0890 (06.03) Negative Beilstein , field identification of coatings, test, 0 5043 (06.01) Neutral salt sprqy test See Salt spray (fog) testing. Newtonian liquids viscosity of paints/vamishes/lacquers, by Ford viscositv cjp, test, 01200 (06.01) viscosity of printing inks/vehicles, by falling-rod viscometer, test, 0 4040 (06,01) Nitration grade/pure benzene/benzol See Benzene Nitration grade/pure toluene/toluol See Toluene Nitration grade xylene See Xylene (nitration grade) Nitrobenzene nitrobenzene in aniline, test, 0 4589 (06.03) Nitrocellulose See Cellulose and cellulose derivatives (headings) Nitrogen-containing plastics nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, 0 1013 (06.02) Nitrogen content nitrogen (total) content of nitrogen-containing plastics/ resins/resin solutions, test, 0 1013 (06.02) soluble cellulose nitrate, testing, methods, 0 301 (06.02) 1168 -- . nitrocelluf 4795 (06;(|" ine base oof. p 4471 (06| fine componl iamine com| S[D 2082 (06 Somatic hyd| Sa Hydro satic hydra D 4790 (0[ jurities in 1 1651,051, fi non-atotj hydrocaif zylenes,] fero0>atic v|j %cmical anf t 0449|| itonducti ffy film the# " nonfetl ,, 0l4|| |conduct||; "ynfinuity | substrt .conducfif iscontiti'f coatijiconjugaf See t I pncontak| tempera)!, curd londestew effect ,,g fj film M l^onde^ttfc Non-hu. *= i Nonleafe| j 1 SIS' ; t; Nonmajfl | Nonrrfi; dwgV DUP050298344 Index of ASTM Standards, Section 6 Nuclear reactor vessels--coatings application^ I soluble nitrocellulose, by ferrous sulfate procedure, test, D 4795 (06.02) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) operating light-/water-exposure apparatus (fluorescent-UV condensation type) for exposure of nonmetallic materials, practice, G 53 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) Non-Newtonian coatings laboratory preparation of gelled vehicles, using microwave oven, practice; D 5166 (06.02) rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) viscosity of paints/varnishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) viscosity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) Nitrogen impurities pyridine base content in cresylic acid, by direct titration, test, D4471 (06.03) Nonamine component content non-amine component content of fatty amines/nonamines, test, D 2082 (06.03) Nonaromatic hydrocarbons Sa Hydrocarbons (headings) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, by gas chromatography, test, D 2360 (06.03) xylene isomer analysis, by gas chromatography, test, D 2306 (06.03) Nonaromatic impurities chemical analysis of benzene, by gas chromatography, test, I D 4492 (06.03) I Nonconductive coatings jjj dry film thickness of nonconductive coatings (applied to Inonferrous metal base), nondestructive measurement, test, D 1400 (06.01) Nonconductive linings continuity verification of liquid/sheet linings applied to concrete I substrates, practice, D 4787 (06.01) I Nonconductive protective coatings I discontinuity (holiday) testing of nonconductive protective I coating on metallic substrates, practice, D 5162 (06.01) 1 Nonconjugated oils--iodine value I: See Iodine value I Noncontact thermometer i temperature of applied coatings on wood products during (he 1 curing cycle, by infraredradiation thermometers, practice, I D 3259 (06.01) 1 Nondestructive evaluation (NDE) 1 effects of outdoor weathering on pipeline coatings, test, I G 11 (06.01) I film thickness of pipeline coatings on steel, nondestructive I measurement, method, G12 (06.01) I Nondestructive evaluation (NDE)--x-ray diffraction | See X-ray diffraction I Npnheat-reactive resins sj: See Resins (headings) Nonvolatile matter content--paints/related coatings/materials acid/amine value of fatty quaternary ammonium chlorides, test, D 2079 (06.03) acid/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) cellulosics/emulsions/fesin solutions/shellac/varnishes, selecting test procedures, practice, D 4209 (06.02) driers/drying oils/naval stores and solvents, selecting test procedures, guide, D 4140 (06.03) nonvolatile and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (06.01) nonvolatile content in sittnes/siloxanes/silane-siloxane blends used in masonry watdr-repellent treatments, test, D 5095 (06.01) nonvolatile content oflatexes, test, D4758 (06.02) nonvolatile content ofresin solutions (in volatile organic solvents), test, D1259 (06.02) printing inks/resin solutions/vehicles, test, D 4713 (06.01) sampling and testing shellSc varnish, 0 1650 (06.02) sampling/testing flaked aluminum powders/pastes, methods, D 480(06.03) varnishes, test, D1644 (06411) volatile/nonvolatile content of paint/related coatings, selection and use of test procedures, guide, D 2832 (06.01) volatile/nonvolatile content (of pigments), selecting test procedures, guide, D 4139 (06.02) volatile organic compounds (VOC) of solvent reducible paints in aerosol cans, test, D 5200 (06.0T) volatile solvents, test, D1353 (06.03) volume nonvolatile matter in dear/pigmented coatings, test, D 2697 (06.01) weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D 3926 (06.02) Notches sag resistance of paints, using a multinotch applicator, test, D 4400 (06.01) wet film thickness of organic coating^, by notched gages, practice, D 4414 (06.01) NPIRI method fineness of grind of printing inks, by NPIRI method, test, D 1316 (06.01) Nuclear paints/related coatings dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) photographic documentation of coatings/lining defects and failures, D4121 (06.01) protective coating/lining work for power generation facilities, terminology, D 4538 (06.01) Nuclear reactor vessels--coatings applications abrading concrete, practice, D 4259 (06.01) acid etching concrete, practice, D4260 (06.01) capillary moisture in concrete, by plastic sheet method, test, D 4263 (06.01) I Non-human control--algae | See Algae | Nonleafing aluminum pigment See Aluminum powder and paste 1169 Nonmagnetic coatings film thickness of pipeline coatings on steel, nondestructive measurement, method, G 12 (06.01) Nonmagnetic organic coatings dry-film thickness of organic coatings, using micrometers, test, D1005 (06.01) Nonmetallic materials accelerated testing of paints/varnishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, D822 (06.01) disbonding characteristics of pipeline coatings, by direct soil DUP0502 98345 burial, test, G 19 (06.01) gloss of high-gloss metallic/nonmetallic surfaces, bygoniophoto- metry, method, E 430 (06.01) operating carbon-arc light-exposure apparatus with and without water for exposure of nonmetallic materials, practice, G 23 (06.01) Index of ASTM Standards, Section 6 Nuclear reactor vessels- -coatings applications coatings' for light-water cooled nuclear power plants, D 3912 (06.01) decontaminability of coatings used in light-water nuclear power plants, test, D 4256 (06.01) design/fabrication of fltle gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) design/use of safety alert system for hazardous work locations in coating/lining industry, practice, A D 4257 (06.01) dry film thickness of protective coating systems, by destructive jneans. test, D4138 (06.01) effects of radiation on coatings (for light-water nuclear power plants), test, 1) 4082 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power-plant, guide, , D 5163 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01): oil/water, presence in compressed air (used for coating, application/air blast cleaning/abrasive blast cleaning), D 4285 (06.01) pH of chemically cleaned/etched concrete surfaces, 04262(06.01) photographic documentation of coatings/lining defects and failures, D 4121 (0601) purity of methyl isobutyl ketone, by gas chromatography, test, 0 3911 (06.01) f quality assurance, practice, 0 3843 (06,01) > >. sample preparation for quafification-testing of coatings (ttsed in nuclear power facilities), spec., 13:5139 (06.01) selecting test methods, guide for, 03842 (06.03) , specifying inspection requirements for coating/lining work on metal substrates, guide, D 5161 (06.01) surface cleaning concrete (for coating), practice, 0 4258 (06.01) surface cleaning concrete unit masonry (for coating), practice, D4261 (06.01) , ,s, use of protective coating standards in nuclear, power plants, selecting ASTM standards, guide, I) |i,44 (06.01) Nuclear reactor vessels--qualifications for painters coating contractor qualification (for nuclear-powered generation facilities), practice, D 4286 (06.01) establishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities, guide, D 4537 (06.01) qualification ofjourneyman painters for application of coatings to concrete surfaces of safety-related areas in nuclear facilities, practice, '04227 (064)1) qualification ofjourneyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities, practice, D 4228 (06.01) jy n o Ocher chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, 0 50 (06.02) ochre pigment, spec., D 85 (06.02) n-Octane purity of hydrocarbons from freezing points, test, D1016 (06.03) Odor field identification of coatings, test, D 5043 (06.01) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) volatile solvents and diluents, test, 0 1296 (06.03) Oil absorption calcium borosiiicate, test, 0 4487 (06.02) pigments, by Gardner-Coleman method, test, D1483 (06.02) pigments, by spatula rub-out test, 0 281 (06.02) Oil acids identification of oils and oil acids in solvent-reducible paints, test 0 2245 (06.03) Oil-base paints | Oils--fat: See Solvent-reducible paints/coatings flash p i, Oil content artists' paints (oil/resin-oil/alkyd), spec., 0 4302 (06.01) oil/water presence in compressed air (used for coatinappiication/air blast cleaning/abrasive blast cieanuiu Pf 1 Oils--lib whitei re 0 4285(06.01) Oils--lu Oil resistance wood furniture lacquers, test, D 2571 (06.01) flash j P Oils Sa Hydraulic fluids Oils--m; miner, coconut oil, spec., 0 1841 (06.03) miner corn oil, spec., 0 1842 (06.03) `5 s cottonseed oil, spec., D1843 (06.03) Oils--o fish oil content (of drying oils a,ud then- fatty ictdsi, gns- liquid chlor< chromatography, test. D 3725 (06.03) ' -1' * gel tii identification ofoils and oil acids in solvent-reducihle i iii,test 0 2245(06.03) rosin oils, testing, 01131 (06.03) safflower oil, spec., D1392 (06.03) m s bitieii Oils--p samp samp sunflower oil (once-refined, technical grade), spec-, 0 3169(06.03) , water in liquid naval stores, test, 0 890 (06.03) Oils--castor dehydrated castor oil, spec., 0 961 (06.03) hydrdxyl value of fattyoifs/Mds, test, 0 1957 (06.03) raw castor oil, spec., 0 960 (06.03) - spectrophotometric diene value of dehydrated castor oil/derivatives, test, 0 1358 (06.03) Oils--drying r acetone tolerance of heat-bodied drying oils,-test,- .. idK watei Oils--! degii ' refu| ons--Sr distil , tail! ' Oils--1 v - oleic voiat; 0 1950 (06.03) ash content, test, 0 1951 (06.03) boiled linseed oil, spec., 0 260 (06,03) break, test, 0 1952 (06.03) Oilsgel't quail color after heating, test, 0 1967 (06,03) color of transparent liquids, by Gardner color scale, test, a: 0 1544 (06101,06.02; 06.03) !' 1 Oily1!21 samt - degummed soybean oil, spec!, D12*4 (06.03) dehydrated castor oil, spec., 0 961 (06.03) drying oils, selecting test methods, guide, 0 555 (06.03) film formation rates in drying or curing piOces$, at robtri' Oleij: i olbii Once# temperature, test, D1640 (06.01) ` -stM fish oil content, by gas-liquid chromatography, test, ' 0 3725(06.03) foots, by gravimetricmethod; test, 0 1966(06103) foots, by volumetric method, test, 0 1954 (06.03) _ gel time, test, 01955 (06.03) iodine value, test, 0 1959 (06.03) ' , ./ Op loss on heating of drying oils, test, 0 1960 (06,03), .. ,, methyl esters, preparation for fatty acid composition analysis by gas-liquid chromatography, 0 2800 (06.03). % oiticia oil (permanently liquid), spec., 0 601 (06,03) raw castor oil, spec., 0 960 (0603) raw linseed oil, spec., 0 234 (06.03) raw turtg oil, spec., D 12 (06.03) Opt# refined soybean oil, spec., 0 1462 (06(03) safflower oil, spec., 0 1392 (06.03) sampling liquid oiis/fatty acids (commonly used in paints/ vamishes/related materials), test, D1466 (06.03) saponification value of drying oils/fatty acids/polymerized fatty acids, test, 01962 (06.03) specific gravity at 25/25C, test, 0 19,63 (06.03) unsaponifiable matter in< drying oils/fatty acids/polymerized fatty acids, test, 0 1965 (06.03) ,, volatile/nonvolatile content (of driers/drying oijs/naval stores and solvents), selecting test procedures, guide, 04140(06.03) Oilsi--fatty clarity/cleanness' of (nonpigmented) paint and ink liquids, by visual examination, test, 0 2090 (06.02, 06.03) 1170 DUP050298346 Index of ASTM Standards, Section 6 Organic linings Oils--fuel flash, point (offuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D93 (06.03) Oils--linseed white-linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (06.01) Oils--lubricating flash point (of fuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) Oils--mineral mineral oil content, of rosin oil, test, D1131 (06.03) mineral (petroleum) spirits hydrocarbon dfyeleaning solvent; > spec., D 235 (06.03) ,v Oils--oiticica chloroform `insoiBbl^hsatter in ditieia oil, test, D1958 (06.03) gel time, test, D`1955 (06.03) '' ! ' ; biticla o'il (permanently !igtiid), spec.', D601 (06.03) - `-! Oils--pine (natural/synthetic) ' - , ; _ sampling and testing `pine drip mefhbti, 0 8'02;(O6.03)' ' sampling/testing pine tars/pine-tar oils, test,;'u 856 (06.03) water in liquid naval' stores, left, B89Q'(06.03) . ` Oils--soybean , _ degummed sdybean oil, spec:; D.124 (06.03) refin'ed soybean oil, spec., D 146.2'(06.03) . \` ., : Oils--tall , ' '1' ; , distitledfattyacids,',spec.;D 1984(06.03)' tall oil, methods of testing Ik 003 (06.03) ~\'` Oils--tall oil rosin". " \ ;i:. oleic acid content pf tab pii rori,ri;'test, p Ii>85 (06.03) volatile resin & tali ofi/gupi/wood *os^,`>y gas. chromatography, test, D 30,08 (06.03)" ` ^ Oils--tang gel time, test, II1955 (06.03), , quality determinafibn, test," D 1964 (06.03) raw pastor oil, spec., D 1.2 (06.03).^ ... )u ' , _, .. Oily matter content ,, , , sampling/testing flaked, aluminum powders/pastes, methods,. D480 (0.6.03) , .T; -. s . .. Oleic acid, content 7 .. . c-wv. is /, . < * oleic acid content of tall oil rosin, test, D1585 (06.03)-, Once-refined sunflower oil (technical-grade), sunflower oil (onpe-refined, technical.gjadp)* spec,,-. ,p D 3169 (06.03) Opacity . , biding poweE of arehitectuml paints applied by roller, test, , . .' 05150 (06.01) - ,, - : ,/ Opacity/opaque materials , > i :>' directional-reflectaiicefactbri-(45-dsg 0"deg) of opaque - - specimens, by broad-band filter refiectometry, test, E97 (06.01) ' ._ testing industrial water-reducibie coatings, guide, 0471\(06.01) Open-cup flash point methods n, ,:-i , : See Flash point (headings) , ,. Optical materials/properties/tests Sa Clarity/cleanness//Gloss/Haze Hiding power/Luminance/Metamerism Reflectance and reflectivity Refractive index/Tihting Strength printing ihks/ink filhis/rfelated materials, selecting test methods, guide, D 5010 (06.01) Orange pigments chrome yellow/orange pigment, spec., D 211 (06.02) molybdate orange pigments, spec, D 2218, (06.02) yellow/orange/green pigments containing, lead chromate/ chromium oxide green, analysis, test, !) 126 (06.02) Orange shellac See Shellac Organic coatings ! c ,* 1 abrasion resistance, by Taber abraser, test, D 4060 (06.01) acid value of organic coating materials, test, D 1639 (06.01) adhesion of organic coatings to plastic substrates, by direct tensile testing, D 5179 (06.01) adhesion, (o smooth panel surfaces, by scrape test, D 2197 (06.01) clear/pigmented organic coatings, test, D1308 (Q6.01) conducting tests on paint/vamish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D5031 (06.01) detergent resistance, practice, p 2248 (06.01) dry-film, thickness of organic coatings, using micrometers, test, D 1005(06101) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) ; effect of staining agents, fdr1 p&dufcts in the transportation industry, practice, D1540 (06.01) effects of overbaking on organic coatings, practice, D 2454 (06.01) evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A D 2485 (06.01) exposure of paints/related coatings to fluorescent UV- ; condensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) filiform corrosion resistance, test, D 2803 (06.01) film formation rates in dfying or curing process, test, D1640 (06.01) film hardness, by pencil test, D 3363 (06.01) flexibility/adhesion of organic coatings (paints) on prepamted deformed metaliic Sheets, test, D 4145 (06.01) formability (of attached coatings), with impact-wedge bend apparatus, test, D 3281 (06.01) ' ' hardness of organic coatings, by Kdnig/Persoz,pendulum hardness tests, D 4366 (06.01) mandrel bend test of attached organic coatings, test, P5?2 (06.01) , moisture vapor transmission of organic coating.films, test, D1653 (06.01) practical wasliability of organic coatings, test, D 4828 (06.01) preparation of free films of organic coatings, practice, D 4708 (06.01) producing films of uniform thickness of paint/vamish/reiated products on test panels, test, D 823 (06.01) resistance of organic coatings to effects of rapid deformation (impact), test, D 2794 (06.01) resistance to pressure mottling and blocking, test, D 3003 (06.01) silicon content of silicone polymers and silicone-modified alkyds, by atomic absorption spectrophotometry, test, D 3733 (06.02) testing finishes on primed metallic substrates for humiditythermal cycle crackingsmethod, D 2246 (C6.01) testing water resistance ofeoatings, using feter-fog apparatus, practice, D1735 (06.01) water immersion test, D 870 (06.01) wet film thickness of organic coatings, D 1212 (06.01) _>yet film thickness of organic coatings, by notched gages, practice, D44I4 (06.01) Organic compounds acrylic acid dimer in acrylic acid/unsaturated organic acids, test, D 4415 (06.03) alcohol-benzene soluble matter in cellulose, test, D1794 (06.02) amount of volatile organic compound (VOC) released from solventbome automotive coatings and available for removal in a VOC control device (abatement), test, D 5087 (06.01) sampling industrial chemicals, practice, E 300 (06.03) trace peroxides (5-80 ppm), using spectrophotometer, test, E 299 (06.03) Organic linings inspection of linings in operating flue gas desulfurization systems, practice, D4619 (06.01) * 1171 I 1 DUP050298347 Index of ASTM Standards, Section 6 Organic liquids (volatile) Organic liquids {volatile) See Volatile organic compounds (VOC) Organic matter content volatile organic content (VOC) of paints/reiated coatings, selecting test procedures, practice, D 3960 (06.01) Organic solvents See Solvents Organotin . organotin release rates of antifouling coating systems in sea . water, using graphite furnace atomic absorption, . spectrophotometry (GP-AAS), test, D 5i08 (06.01) Orpiment content sampling/testing lac resins (orange sheilac/button lac/gamet lac/bleached lac), test, -D 29 (06.02) Orthoxylene See ortho-Xylene Outdoor weathering See Weathering--outdoor Ovens nonvolatile opntent of printing inks/resih solutions/vehicles, test, D 4713 (06.01) Overbaking (of paints/related coatings) , effects of overbaking on organic coatings, practice, D 2454 (06.01) Oxidative microcoulometry sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, D 3961 (06.03) Oxirane epoxy content of epoxy resins, test, D1652 (06.02). Oxygen (active) content See Active oxygen content Oxygen degradation , conducting tests on paint/vamish/Iacquer/related products, using enclosed carbon-arc ilght/vvatef exposure apparatus, practice, D5031 (06.01) exposure ofpaints/reiated coatings to fluorescent UV- condensation light-water-exposure apparatus, practice fdr conducting tests, D 4587 (06,01) P Package stability estimating package stability of coatings for ultraviolet curing, test, D 4144 (06.01) freeze-thaw resistance of water-borne Coatings, test, D2243t06.01) package stability of solvent-reducible/water-reducible paint, test, D1849 (06.01) resistance of emulsion paints (in containers) to attack by microorganisms, test, 0 2574 (06.01) ' sampling liquid paints/reiated pigmented coatings, practice, D3925 (06.01) Packaging and packaging materials abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) Paint--architectural See Architectural coatings Paint--automotive See Automotive coatings/paints Paint--chromatic See Chromate coatings Paint--curing See Curing characteristics Paint--general acidity in volatile solvents/chemical intermediates (used in paint/varnish/lacquer/related products), test, D1613 (06.03) clear/pigmented organic coatings, test, D1308 (06.01) conducting tests on paint/varnish/lacquer/reiated products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) dichloromethane/l.U-trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, D 4457 (06411) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter'reflectometry, test, E 97 (06,01) dry-film thickness of organic coatings, using micrometers, test, D1005 (06.01) erosion testing of antifouling paints, using high velocity water, test, D 4938 (06.01) . evaluating degree of settling (pigment suspension/easp of remixing a shelf-aged sample) ofpaint, test, D 869 (06.01) evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A D 2485 (06.01) field identification of coatings, test, D 5043 (06.01) fire retardancy ofpaints, by cabinet, method, test, A D1360 (06.01) ' fiasli/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) ,, ' _ , flash point by Tag closed tester, test, D 56 (06.03) index of ASTM methods equjvajent/refated to methods,in, Federal Standard 141 ("Paint, Varnish, Lacquer, and Related Materials; Methods for Sampling and Testing"), (Related Material) (06.01,06.02, 06,03) index ofstandards by ISO/TC 35 on Paint' and Varnishes, (Related Material) (06.01, 06.02, 06.03) paint/vamish/Iacquer/related products, terminology, ' D 16 (06.01, 06.02, 06.03) ; / preparation of free films of organic coatings, practice,'' D 4708 (06.01) recording results on single-/multi-panel forms, method, A D1150 (06.01) small-scale evaluation of fire-retardant paints, by 2-foot tunnel method, test, D 3806 (06.01) standard environments for conditioning/testing paint/ vamish/lacquer/related materials, spec.,' 0 3924 (06.01) titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D 4764 (06.01) wet film thickness of organic'Coatings, D1212 (06.01) Paint--industrial water-hnse c,; ^ pigment content, by low temperature ashing, test, D 3723 (06.01) testing industrial water-reducible coatings, guide, D 4712 (06.01) testing water resistance of coatings at 100 % relative humidity,~ practice, D 2247 (06.01) ___ , water content ofyvaten-redtidible paints, by direct injection into gaschromatograph, test; B 3792 (06.01) Paint--inspectors Sa Qualifications " painting inspectors (metal substrates), guide, D 3276 (06101) Paint--latex See Latex paints Paint--primer See Primer '` Paint--selection/use of test procedures See Guides fqr testing paints/reiated coatings/materials Paint--solvent-reducible See Solvent-reducible paints/coatings Paint--thinners ester value of solvents and thinners, test, D 1617 (06.03) evaporation rate, test,: D 3539 (06.01) nature ofthinners in solvent-reducible paints, qualitative determination, method, D 2349 (06.01) Paint brushes preparation of paint brushes for evaluation, practice, D 5068 (06.01) 1172 Paint r ! prepi: Paint s pain Paint t recq Pale g i. Panel : eval mar Panel recc ` Panel: woe PapeJ din DUP050298348 Index of ASTM Standards, Section 6 Petroleum/petroleum products Paint roller preparation of paint roller covers for evaluation, D 5069 (06X1) Paint spatter resistance paint spatter resistance to roller application, test, D 4707 (06.01) Paint test results recording results on single-/multi-panel forms, method, A D1150 (06.01) Pale gold bronze See Gold bronze powder Panel evaluation evaluation of painted/coated specimens subjected to corrosive environments, method, 01654 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) Panel forms recording results on single-/multi-panel forms, method, A D 1150 (06.01) ' Panels wood used as panels in 'weathering tests of coatings, si>ec'., D 358 (06.01) Paper and paperboard directional reflectance factor (45-deg 0-deg) ofopaque specimens, by broad-band filter reflectometry, test, 97(06.01) lightfastness of printed matter, D3424 (06.01) Para (paranitraniline) red Sir Pigments (generalproperties) pure para red toner pigment, spec., D 475 (06.02) Para red pigment para redApluidine red pigments, testing, D 970 (06.02)' Paraxylene See para-Xylene Paris red See Red lead Paris white See Calcium carbonate Paris yellow See Chrome yellow and orange Particle size (analysis/distribution) chemical analysis of calcium borosilicate, test, D 4487 (06.02) coarse particles in pigments/pastes/paints, test, D185 (06.01, 06.02) . multicolor lacquers, test, A D 2338 (06.01) polymeric powder properties, by multiple sieve method, practice, D 3451: (06.01) reporting particle size characteristics of pigments, practice, D 1366 (06.02) Particle size (analysis/distribution)--distribution particle size distribution, by hydrometer of'common white extender pigments, test, D 3360 (06.02) Paste coarse particles in pigments/paste^/paints, test, D185 (06X1, 06.02) Pastes in oil (of pigments) See Pigment dispersions (paint)--white pigment analysis Patches comparative corrosion preventive characteristics of materials used for joints/coupiings/fitfings/patches in pipeline coatings, test, G 18 (06.01) Patch test conducting a patch test to assess coating compatibility, practice, 05064(06.01) Pavement marking paint See Traffic paint Peen plating See Coatings--mechanically deposited Pencil test film hardness of organic coatings, test, D 3363 (06,01) Pendulum test hardness of organic coatings, by Konig/Persoz pendulum hardness tests, D4366 (06.01) Penetration--paint film porosity of paint films (to indicate coating penetration), test, D 3258 (06.01) Penetration--pipeline coatings impact resistance of pipeline coatings, by falling weight test, G14 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) Pensky-Martens closed tester Sa Flash point (headings) flash point (of fuel oils/lube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) Pentaerythritoi giyceroi/ethylene glycoi/pentaerythritol in alkyd resins, test, D1615 (06.02) pentaerythritoi (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) Pentane purity of hydrocarbons from freezing points, test, D 1016 (06.03) Pentosans content ' pentosans content of cellulose, test, D1787 (06.02). Percent dilutabillty resin solution dilutability, test, D 5062 (06.03) Percent epoxide epoxy content of epoxy resins, test, D1652 (06.02) Performance--coatings clear floor sealers, D 1546 (06.01) establishing procedures to monitorperformance of safety related coatings in operating1 nuclear power plant, guide, D 5163 (06.01) subjecting marine antifouling coating to bifoufing and fluid shear forces in natural seawater, test, D 4939 (06.01) Performance--nuclear materials/applicadons establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, D 5163 (06.01) Permanent white See Barium sulfate Permanganate time permanganate time of acetone/methanol, test, 01363, (06.03) tricresyl phosphate, test, D1721 (06.03) Permeability--films moisture vapor transmission of organic coating films, test, D 1653 (06.01) Permeability absorption --,, reporting partide size characteristics of pigments, practice, 0 1366(06.02) Permeance moisture vapor transmission of organic coating films, test, D1653 (06.01) Peroxides Sa Active oxygen content peroxides in styrene monomer, test, D 2340 (06.03) trace peroxides (2:5-80 ppm), using spectrophotometer, test, E 299 (06.03) Persian gulf oxide See Iron oxide red Persoz pendulum test hardness of organic coatings, by Konig/Persoz pendulum hardness tests, D4366 (06.01) Petroleum--mineral spirits See Mineral spirits Petrolenm/petroleum products cresylic acid content (of alkaline cresylate solutions), chemical analysis, D 3439 (06.03) 1173 DUP050298349 Index of ASTM Standards, Section 6 Petroleum/petroleum products--distillates Petroleum/petroleum products--distillates water in petroleum products/bituminous materials, by distillation, test, D 95 (06.01, 06.03) Pfund indentation hardness Sa Hardness tests--organic coatings indentation hardness of organic coatings, by Knoop and Pfund methods, test, D1474 (06.01) Pfund wet film thickness gage wet film thickness of organic coatings, D 1212 (06.01) pH Sa Acidity, alkalinity, pH (headings) apparent pH of electrocoat baths, test, D 4584 (06.01) apparent pH of water insoluble phenol-formaldehyde resin, test, D4613 (06.02) pH of chemically cleaned/etched concrete surfaces, D 4262 (06.01) Phenol analysis of major organic impurities in phenol produced by the cumene process, by gas chromatography, test D 4961 (06.03) and cresylic acid, sampling and handling, practice, D 3852 (06.03) apparent free phenols, in synthetic phenolic resins/solutions (used in paints/related coatings), test, D 1312 (06.02) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) color of cresylic acids ("C" series standards), test, D 3627 (06.03) phenol content of (refined) isopropylbenzene (cumene), test, D 3160 (06.03) phenol content (of tar acid mixtures), by gas liquid chromatog raphy, test, D 3626 (06.03) refined phenol, spec., D 2439 (06.03) water content, by iodine reagent method, test, D1631 (06.03) Phenolic resins Sa Resins (headings) apparent free phenols, in synthetic phenolic resins/solutions (used in paints/related coatings), test, D1312 (06.02) apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (06.02) methylol group determination (qualitative) in phenolic resins, test, D 4706 (06.02) stroke cure time of thermosetting phenol-formaldehyde resins, : test, D 4640 (06.02) volatile content in phenolic resins, test, D 4639 (06.02) Phosphorus acid content zinc hydroxy phosphite, test; D 4450 (06.02) ` Photographic processing photographic documentation of coatings/lihing defects and failures, D 4121 (06.01) Photographic standards for surface preparation standard pictorial surface preparation standards fpr painting steel surfaces, A D 2200 (06.01) Photometry directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, 97(06.01) gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) Phthalate ester color pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) Phthaiic anhydride color in molten state/after heating, by platinum cobalt scale (includes maleic anhydride), test, D 3366 (06.03) sampling and handling aniline, practice, D 3438 (06.03) Phthaiic anhydride--refined refined phthaiic anhydride-1308, spec., D 2403 (06.03) Phthaiic anhydride content alkyd resins/resin solutions in absence of dibasic acid< D 563 (06.02) alkyl resins/resin solutions containing dibasic acids by gravimetric test, D 1306 (06.02) Phthalocyanine blue chemical analysis of phthalocyanine blue/guut pigm/nK test D 3256 (06.02) Phthalocyanine green chemical analysis of phthalocyanine blue/green pigments test ,D 3256 (06.02) '' Phthalocyanine (phthalo) blue chemical analysis of (iron/copper phthaiocv-niiie/ullrdmaune) blue pigments, test, Dl135 (06.02) copper phthalocyanine blue pigment, spec., D 963 (0b.02) Phthalocyanine (phthaio) green phthalocyanine green pigment, spec., D 3021 (06.02) Physical constants calculating formulation physical constants of paints/comings practice, D 5201 (06.01) Physical strength/resistance (nonchemical) printing inks/ink films/rglated materials, selecting test methods guide; D 5010 (06.01) Pictorial surface preparation standards Sa Surface preparation [headings) standard pictorial surface preparation standards for painting . steel surfaces, A D 2200 (06.01) Pigment analysis See Pigments (general properties) Pigment bleeding test bleeding characteristics, of dry pigments, test, D 279 (06.02) > Pigment content antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (06.02) moisture content of pigments, D1208 (06.02) * nonvolatile and pigment content of electrocoat baths, using muffle furnace, test, D 5145 (06.01) paint/traffic marking material, by low-temperature furnace asbing, test, D 4451 (06.01) pigment content of solvent-reducible paints, test, D 2371 (06.01) sblvent-reducible paints, by high-speed centrifuging, method, D 2698 (06.01) sulfide in white pigment separated from solvent-reducible paints, test, D 2351 (06;02) sulfur dioxide' in white pigment separated from solvent- ' reducible paints, test, D 2352>(06.02) titanium dioxide content of jjigments (recovered from whole ~ paint), by atomic absorption spectroscopy, test, D 4563 (06.01) vacuum distillation (for vehicle separation in solvent-type paints), practice, D 3272 (06.01) vehicle separation from solvent-reducible paints, by centrifuge, practice, D 2372 (06.01) water-based paints, by low temperature ashing, test, D 3723 (06.01) water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) Pigment dispersion (paint) Sa Pigments (general properties) antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (06.02) coarse particles in pigments/pastes/paints, test, D 185 (06.01, 06.02) evaluating degree of settling (pigment suspension/ease of remixing a shelf-aged sample) of paint, test, D 869 (06.01) fineness of dispersion of pigment-vehicle systems, test, D1210 (06.01) fineness of grind, printing ink, test, D 1316 (06.01) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, D 2621 (06.01) 1174 particle ex weight pil white 1: Pigment relativ Pigment| lead/cf cl si Pigmentj volui Pigmenn ` alum# Pigment alunti anl hydr|; Pigme| baritf sol# Pigmer basic! whiti r Pigmer bait chfo Pigm whit Pigme' irbn h. solv Pig DUP050298350 Index of iM'lM < L< < J<1' S-\ ion * Pigments--phthalocyanine blue particle size distribution, by hydrometer of common white extender pigments, test, D 3360 (06.02) weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D 3926 (06312) white linseed oil paints- chemical analysis, selecting test methods, practice, 0 215 (06,01) Pigment dispersion (paint) relative tinting strength of printing ink dispersions, test, , D 2066 (06.01) Pigment dusts . lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4338 (06.02) Pigmented coatings volume nonvolatile matter in clear/pigmented coatings, test, D 2697 (06.01) Pigments--aluminum, powder and paste aluminum powder/paste pigments for paints, spec., D 962 (06.02) Pigments--aluminum silicate aluminum silicate (hydrous/anhydrous) pigment, analysis, test, D 718 06.02) anhydrous, spec., D 3619 (06.02) hydrous, spec., D 603 (06.02) Pigments.--barium sulfate barium sulfate pigments, spec., D 6fi2 (06.02) solar energy transmittance test of glass-fiber-reinforced plastic panels, annex D 715 (06.02) Pigments--basic carbonate white lead basic carbonate white lead pigment, spec., D81 (06.02) white lead- chemical analysis, test, 01301. (06.02) Pigments---basic lead silicochromate basic lead silicochromate pigment, spec,, 01648 (06.02) chromium trioxide content of basic lead silica-chromate pigment, test, D1844 (06.02) Pigments--basic sulfate white lead white lead- chemical analysis, test, D1301 (06.02) Pigments--black iron oxide black (natural)- chemical analysis, test, D 3872 (06.02) solvent extractable material in black pigments, test. D 305 (06.02) Pigments--bone black bone black pigment, spec., D 210 (06.02) solvent extractable material in black pigments, test, D 305 (06.02) Pigments--calcium borosilicate analysis, 0 4487 (06.02) 'calcium borosilicate pigments, spec., D 4288 (06.02) Pigments--calcium carbonate , calcium carbonate pigment, spec., D 11&9 (06.02) Pigments--carbon black carbon black pigment for paint, spec., 0 561 (06.02) solvent..extractable material in black pigments, test, D 305 (06.02) Pigments--chrome green chrome green pigment, spec., I> 212 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Pigments--chrome yellow and orange chrome yellow/orange pigment, spec., D 211 (06.02) yeUow/orattge/greeri pigments containing lead chromate/ chromium oxide green, analysis, test, D 126 (06.02) Pigments--chromium oxide green chrome oxide green pigment, spec., D 263 (06.02) yeliow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test; D 126 (06.02) Pigments--copper powder chemical analysis of cuprous oxide/copper pigments, test, D 283 (06.02) copper powder (far antifouling paints), spec., D 964 (063)2) Pigments--cuprous oxide , . chemical analysis of cuprous oxide/eoppenpigments, test, D283(06.02) ' >?," cuprous oxide (forantifouling paints),-spec,, 0 912 (06.02) Pigments--ferrous ochre pigment, spec., D 85 (06.02) Pigments--gold bronze powder chemical analysis ofcuprous oxide/copper pigments, test D 283 (06.02) gold bronze powder, spec., D 267 (06.02) Pigments--iron blue chemical analysis of (iron/copper phthaloryanine/ultramarine) blue pigments, test, D1135 (06.02) iron blue pigment, spec., D 261 (06.02) Pigments---Iron oxide black (natural/synthetic) " */ iron oxide black (natural)-chemical analysis, test, D3872 (06.02) Pigmentsi--iron oxide black (synthetic) black synthetic iroD oxide pigment, spec., D 769 (06.02) Pigments--iron oxide brown (natural) analysis, D 50 (06.02) iron oxide black (natural)- chemical analysis, test, D 3872 (06.02). . natural red/brown iron oxide pigments, spec., D3722 (06.02) Pigments--iron oxide brown (synthetic) analysis, D 50 (06.02) synthetic brown iron oxide pigment, spec., D 3724 (06.02) Pigments--iron oxide red (natural) analysis, D 50 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) Pigments--iron oxide red (synthetic) analysis, D 50 (06.02) synthetic red iron oxide pigment, spec., D 3721 (06.02) Pigments--iron oxide yellow analysis, D 50 (06.02) yellow iron oxide (hydrated), spec., D 768 (06.02) Pigments--lampblack lampblack pigment, spec., D 209 (06,02) solvent extractable material in black pigments, test, D 305 (06.02) Pigments--lead chromate chemical/gravimetric analysis ofwhite/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) Pigments--leaded zinc oxide analysis ofwhite zinc.pigments, test, D3280 (06.02) Pigments--magnesium silicate magnesium silicate pigment, analysis, test, D 717 (06.02) -- magnesium silicate pigment (talc), spec., D 605 (06.02) Pigments--mercuric oxide analysis, D 284 (06,02) mercuric oxide for use in antifouling paints, spec., D 911 (06.02) Pigments--mica grit content of mica pigment, test, D 716 (06.02) wet ground mica pigments, spec., D 607 (06.02) Pigments--molybdate orange molybdate orange pigments, spec., 0 2218 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Pigments--ocher analysis, D 50 (06.02) ochre pigment, spec,, D 85 (06.02) Pigments--para red para red/toluidine red pigments, testing, 0 970 (06.02) pure para red toner pigment, spec., D 475 (06.02) Pigments--phthaiocyanine blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, 01135 (06.02) 1175 SI * * .- DUP0502 98351 Pigments--phthaiocyanine blue Index of ASTM Standards, Section 6 copper phthaiocyanine blue pigment, spec., D 963 (06.02) Pigments--phthaiocyanine green chemical analysis: of phthaiocyanine blue/green pigments, test, D 3256 (06.02) phthaiocyanine green pigment, spec., D 3021 (06.02) Pigments--pumice pumice pigment, spec., D 867 (06.02) Pigments--red lead lead peroxide/true ted lead content of dry red lead pigments, test, D 49 (06.02) red lead pigment, spec., D 83 (06.02) Pigments--sienna, burnt and raw analysis, D 50 (06.02) raw/bumt sienna pigments, spec., D 765 (06.02) Pigments--silica diatomaceous silica pigment, analysis, test, 0 719 (06.02) Pigments--silica, diatomaceous diatomaceous silica pigment, spec., 0 60,4 (06.02) Pigments--strontium chromate chemical analysis of strontium chromate pigment, test, D 18(45 (06.02) strontium chromate pigment, spec., D 1649 (06.02) Pigments--titanium dioxide chcmical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and ,, titanium dioxide, test, D 4797 (06.01) . ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, 0 3720 (06.02) titanium dioxide content of pigments (recovered from whole paint), by atomic absorption spectroscopy, test, 0 4563(06.01) titanium dioxide pigments, spec., D 476 (06,02) white titanium pigments, chemical analysis, test, D1394 (06.02) Pigments--toluidinered para red/toluidine red pigments, testing, 0970 (06.02) pure toluidine red toner, spec., D 656 (06.02) , Pigments--ultramarine blue chemical analysis of (iron/copper phthalocyanine/ultramarine) blue pigments, test, 01135 (06.02) ultramarine blue pigment, spec., 0 262 (06.02) Pigments--umber, burnt and raw analysis, 0 50 (06.02) raw/bumt urhber pigments, spec., 0 763 (06.02) Pigments--Venetian red chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) Pigments--white analysis of white zinc pigments, test, 0 3280 (06.02) antimony oxide content of white pigment (separated frbna solvent-type paints), test, D 2350 (06.02) chemical analysis of white pigments, selection of test methods, guide, 034 (06.02) particle size distribution, by hydrometer of common white extender pigments, test, 0 3360 (06.02) ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, 0 3720 (06.02) relative timing strength of white pigments, by reflectance measurements, test, D 2745 (06.02) relative tinting strength ofwhite pigments, by visual observation, test, O 332 (06,02) sulfide in white pigment separated from solvent-reducible paints, test, 0 2351 (06.02) sulfur dioxide in white pigment separated from solventreducible paints, test, 0 2352 (06.02) white lead- chemical analysis, test, D1301 (06.02) white linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (06.01) white titanium pigments, chemical analysis, test, 0 1394 (06,02) zinc oxide pigments, spec., 0 79 (06.02) Pigments--zinc chromate analysis, D 444 (06:02) zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Pigments--zinc dust analysis, 0521 (06.02) zinc dust pigment, spec., O 520 (06.02) Pigments--zinc hydroxy phosphite analysis, 04450 (06.02) zinc hydroxy phosphite pigment, spec., 0 4462 (06.02) > :** figments--zinc oxide analysis of wMte zinc pigments, test, D 3280 (06.02) zinc oxide pigments, spec., 0 79'(06.02) Pigments--zinc sulfide analysis of white zinc pigments, test, D 3280 (06.02) Pigments (general properties) Sa Pigment content artists' acrylic emulsion paints, spec., D 5098 (06.01) artists' paints (oil/fesm-oil/alkyd), spec., D 4302 (06.01) bleeding characteristics, of dry pigments, test, 0279 (06.02) chemical analysis of yellow/orange/fid/brpwfl pigments cbntaining iron/maganese, test, D 50 (06.02) coarse particles in pigments/pastes/paints, test, 0185 (06.01; 06.02) - common properties of pigments, test, D1208 (06.02) evaluation of (clear/pigmented) coatings for rigid/semirigid plastic substrates, practice, 0 3002 (06.01) field identification of coatings, test, 0 5043 (06.01) fineness of dispersion ofpigmerit-Vehicle systems, test, 01210(06.01) ? hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, 0 280 (06.02) lightfastness of pigments (in artists? paints), test, D 4303 (06.01) oil absorption; by Gardner-Coleman method; test, - 0 1483 (06.02) oil absorption, by spatula rub-Out, test, 0 281 (06.02) particle size- fineness of grind- printiiig'inks, test, 01316 (06.01) relative tinting strength of chromatic paints, test, D 4838 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, 0 2745 (06.02) reporting particle size characteristics of pigments, practice, D1366 (06.02) specific gravity, test, 0 153 (06.02) tinting strength/color of colored pigme.nts, by mechanical muller, test, D 387 (06.02) tinting strength/color of colored pigments, by miniature sandmill, test, A 0 3022 (06.02) volatile/nonvolatile content (of pigments),.selecting test " procedures, guide, 0 4139. (06.02) . water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, 0 2448 (06.02) white linseed oil paints- chemical analysis, selecting test methods, practice, D 215 (0,6.01) yellow/orange/green pigments contenting lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Pigments (general properties)--dispersions Sa Pigment dispersion (paint) . evaluating degree of settling (pigment suspensioh/ease of remixing a shelf-aged sample) of paint, test, 0 869 (06.01) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, D 2621 (06.01) particle size distribution, by hydrometer ofcommon white extender pigments, test, 0 3360 (06.02) Pinene sampling and testing turpentine, method, D 233 (06.03) Pinene--alpha and beta wood, gum, and sulfate turpentine, by gas chromatography, test, 0 3009(06.03) Pine tars/pine.tar oils sampling and testing pine oil, method, O 802 (06.03) 1176 sa w Pint Cl r< Pip c c c- Pie < I! W DU P050298352 Index of ASTM Standards, Section 6 Polyurethane raw materials sampling and testing pine tars/pine-tar oils, method, 0856(06.03) water in liquid naval stores, test, D 890 (06.03) Pinhole test continuity verification of liquid/sheet linings applied to concrete substrates, practice, D 4787 (06.01) reposting paint film failure characteristic of exterior latex paints, classification, f> 1848 (0601) Pipeline coatings cathodic disbonding of pipeline coatings, accelerated,proceduve, test, G 8 (06.01) chemical resistance of pipeline coatings, test, G 20 (06.01) comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patehes in pipeline coatings, test, G 18 (06.01) disbonding (cathodic), for pipe coatings subject to elevated/ cyclic temperatures, G 42 (06.01) disbonding characteristics of pipeline coatings, by direct soil burial, test, G 19 (06.01) 4 effects of outdoor weathering on pipeline coatings, test, G11 (06.01) film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) impact resistance of pipeline coatings, by falling weight test, G14 (06.01) impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) ; resistance of steel pipeline coatings to abrasion, by slurry of coarse abrasive/water, test, G 6 (06.01) specific bendability of pipeline coatings, test, G10 (06.01) water penetration unto pipeline coalings, teit, G 9 (06.01) Plasticizer grade alcohol C4-CI3 alcohol, chemipal/fihysical analysis (sfdecltion/bSe of test procedures), E 852 (06313) Plasticizers plasticizer ri>igratioii:from vinyl fabrics to lacquers, method, D 2199 (06.01) Plasties (general) directional reflectance factor (45-dcg 0-deg) of opaque specimens, by broad-band, filter reflectometry, test, E 97 (06.01) ` evaluation of (clear/pigmenred) coatings for rigid/semirigid plastic substrates, practice, D 3002 (06.01) methylol group determination (qualitative) in phenolic resins, test, D 4706 (06.02) nitrogen (total) content of nitrogen-containing plastics/ resins/resiri solutions,`test, D1013 (06.02) operating light-/watetr,exposure. apparatus (fluoresce'nt-UV condensation type) for exposure of nonmetallic materials, practice, G 53 (06.01) volatile content in phenolic resins, test, D 4639 (06.02) Plastic sheet and film paint spatter resistance to roller application, test, D 4707 (06.01) Plastic sheet method capillary moisture in concrete, by plastic sheet method, test, D 4263 (06.01) Plastics (thermoplastic) bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (06.01) evaluation ofcolor for thermoplastic traffic marking materials, test, D 4960 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Plastics (thermosetting) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Platinum-cobalt scale Sa Color (headings) color of clear liquids, test, 01209 (06.01, 06.03) color of maleic/pbthalic anhydride, in the molten state and after heating, test, D 3366 (06.03) color of solid aromatic hydrocarbons, in the molten state, test, D1686 (06.03) solution color of 4,4'-isopropylidenediphenol (dissolved in methanol), test, 0 4789 (06.03) Point impact impact resistance of pipeline coatings, by falling weight test, G14 (06.01) Polarographic methods nitrobenzene in aniline, test, D 4589 (06.03) Polishes amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, 0 4948(06.01) Polycyclic hydrocarbons See Hydrocarbons (headings) Polyester resins identification of carboxylic acids in alkyd resins D 2455 (06.02) identification of pplyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) isophthalic acid content ofalkyd/polyester resins, test, 0 2690(06.02) Polyhexafluoropylene (FEP) substrate preparation of free films of organic coatings, practice, D 4708 (06.01) Polyhydric alcohol identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) polyhydric alcohols in alkyd resins, qualitative analysis, test, D 2998 (06.02) Polymer content polymer content of styrene monomer, test, Q:2121 (06.03) qualitative identification of polymers in emulsion paints, by., infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) ^ Polymeric powders/powder coatings ' selection/use of test procedures, practice, D 3451 (06.01) Polymerization. cellulose nitrate, test, D1716 (06.02) sampling and testing turpentine, method, 0 233.f06.03) unreacted mpnomer content of latexes, by gas-liquid chromatography, test, 04747 (06.02) Polymerization inhibitors p-rert-butylcatechol (TBC) in styrene monomer, test,1 --- 0 2120 (06.03) ..._ Polymerized fatty acids See Fatty acids--tests Polymer latexes Sa Latex paints filter-retained solids contenl of polymer latexes, test, 0 5097 (06-02) Polymers polymer content of styrene monomer, test, D 2121 (06,03) polymerization time of shellac (used for electrical insulation), test, D 411 (06.02) qualitative identification ofpolymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.01) silicone polymers- silicon content, by atomic absorption spectrophotometry, test, 0 3733 (06.02) solubility range, test, 0 3132 (06.02) Polyol acetates identification of polyhydric alcohols in alkyd resins, qualitative/quantitative analysis, test, 0 2456 (06.02) Polyurethane raw materials See Urethanes--polyurethane raw materials (headings) mi PI DUP050298353 Index of ASTM Standards, Section 6 PoIy(vinyl acetate) coating systems Poly(vinyI acetate) coating systems water content of water-reducible paints, by direct injection into gas chromatograph, test, D 3792 (06.01) Poly(vmylbutyral) resins Sa Resins (headings) poly(vinyl butyral)-'chemical analysis; test, D1396 (06.02) Poly(vinyl chloride)(PVQ plastics--resins poly(vinyi chloride) resins, selecting test procedures, guide, D 4368 (06.02) residual vinyl chloride monomer content of poly(vinyl chloride) resins/compounds/copolymers by solution injection technique, test, D 3680 (06.02) Ponderosa pine wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Porcelain enamel products ,, directional reflectance factor (45-deg O-deg) of opaque specimens, by broad-band filter reflectometry, test, E97 (06.01) ; 1^ Porosity--coating porosity of paint films (to indicate coating penetration), test,' D 3258 (06.01) Portable adhesion testers pull-off strength of coatings, using portable adhesion testers,, test, D 4541 (06.01) Potash blue See Iron blue , . ,. Potassium permanganate reduction See Permanganate time Potentiometric method acid number of rosin, test, D 465 (06.03) maleic acid content of maleic anhydride, by potentiometric ' titration, test, D 2930 (06.03) saponification number of rosin, test, D 464 (06.03) * Powdered chemicals' directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, tost, E 97 (06.01) Power generating facilities design/fabrication of flue gas desulfurization system components (for protective lining application), spec., D 4618 (06.01) dry film thickness of protective coating Systems, by destructive means, test, 1)4138 (06.01) inspection of linings inoperating flue gas desulfurization' systems, practice, D 4619 (O6;01) photographic documentation of coatings/lining defects and failures, D 4121 (06.01) J protective coating/lining work for power generation facilities, terminology, D4538 (06.01) Power law viscosity of printing inks/vehicles, by falling-rod viscoiheter, test, D 4040 (06.01) Power tool cleaning standard pictorial surface preparation standards for painting steel surfaces, A D 2200 (06.01) Precautionary labeling ' labeling art materials for chronic health hazards, practice, D 4236 (06.01) Precision conducting interlaboratory study to determine precision of test method, practice, E 691 (06.03) Precision--instrumentation directional reflectance factor (45-deg. 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) Preformed tape (for traffic marking) pigment content of paint/traflic marking,material, by iow-temperature furnace ashing, test, D 4451 (06.01) Pregel vehicle r., . laboratory preparation of gelled vehicles, using iaicroreiXv I practice, DS166 (06s02) uwws aven, Preparing specimens (for testing) See Specimen preparation (for testing)(te.rfi/,*,, Prepolymers <,, isocyanate group content of urethane materials/nieroKri -r, test, D 2572 (06.02) 1` Pressure mottling pressure mottiing/blocking resistance of oiganic coalings fon metal substrates), test, D 3003 (06.01) Primary amylacetate v.i , See jAmyl.itoqta'te ' Primary hydroxyl content J primary, hydroxyl content of cellulose acetate, test D 871 (06.02) primary hydrqxyl.content of cellulose esters, test, A D 817 (06.02) . Primer , formability/adhesion ofzinc-rich primer/chromate; complex coatingsfon steel), test, D4146 (06.01) ,, , > >; MEK resistance of ethyl-silicate (inorganic) zinc-rich primers by solventTUb; test, D4752 (06.01) testing primers/primer surfecers over preformed metal; selecrion/use df procedures, practice, D 3322 (064)1) zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Primrose chrome/yellow See Chrqme yellow and orange ; ! Printed matter ,, . . . abrasion resistance of printed..matter, by,the ga-'cat comprehen sive abrasion test, )>'181 (09 )1) method for evaluating lightfastness. b3424 (06.01) * Printing ink resins , r : .. ; v""1 resin solution dflutabifityl test, ,D, 5062 (06.03). . Printing inks abrasion resistance :0;f panted matter, by thega-cat compreBeh- * sive abrasion test, D 5181 (06.01) ' ' apparent tack of printing inks/vehicles, by inkometcr, test, D 4361 (06.01) ' commercial hexanes, spec., D' lj)36 (06.03) "J fmeness'Ofgrind of printingiriks^ tty ftPIRI method', test D1316 (06.01) "" ' nonvolatile content Sfpnfltlhg mte/tosih solutidns/vehiblfes,' test, D4713 (06.01) ' ;.'* f printing inks/irik films/related materials!, selecting test methoils, guide p 5010 (06.01) * ' ;)L' : : , - relative tmtingsttenj^df prihtittgiiifc cfisfiet's'tons, test, 1 D 2066 (06.01) '-- viscosity of printing inks/vehicles, by falling-rod viscometer; test, 1)4040 (06.01) water pickup of lithographic printing inks/vehicles in'a , laboratory irfixer, test, D 4942 (06.01) Printing substrates ; printing ihks/ihk filffis/telafed materials, selbcfing tdst rmefhods, guide, D 5010 (06.01) Print resistance f` print resistance of architectural paints, test, D 2064 (06.01) Print resistance of lacquers , See Lacqiier.' !: . '' Procedures . .. estabiishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities,,guide, p 4537 (06,01) Production method , o' transfer efficiency under production conditions for spray. application of automotive paints, by weight, basis, practice, D 5066 (06.01) ........ 2-Propanone. See Acetone ut ,- i Propionyl ct acetyl ant test. n-Propylto alcohol c test, n-propyl n-Propyl a! n-propyl ; Propylene propylet t prOpylei t Propylene f propyle D purity c mi ac Propylen propyl Protectii analw A proteji pull-bt. use jaf Protethf hand! adh bolt Pur 4 1178 DUP050298354 * .* 11. Index of ASTM Standards, Section 6 Quality assurance Hfel <wWfcto tafflfc a ft -^``r fflij. |9 ,2mi,li>*sVMj, iMEgl 't o r I m* Propionyl content I acetyl and propionyl/butytal contents of cellulose mixed esters, test, A D 817 (06,02) u |-Propyl acetate ' alcohol content/purity of acetate esters, by gas chromatography, test, D 3545 (06.03) i n-propyl acetate (96 % grade), spec.; D 3130 (06.03) i-Propyl alcohol n-propyl alcohol (1-propanol), spec., D 3622 (06.03) Propylene glycol R' propylene glycol/dipropylene glycol, spec., D 5164 (06.03) propylene glycol, spec., D 2695 (06.03) topylene glycol nionomethyl ether acetate (PMA) propylene glycol monomethy! ether acetate, spec., D 4835 (06.03) purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03)' Propylene glycol monomethyl ether (PM) propylene glycol monomethyl ether, spec., D4837 (06.03) purity ofpropylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethy] ether acetate, test, D 4773 (06.03) `rotcctire coatings analytical procedures for determining hazardous constituents'in protective coatings, selecting test methods, guide, ' D 3630 (06.01) protective coating/lining work for power generation facilities, terminology, D 4538 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) protective equipment handling/sampling phenol and cresylic acid, practice, D 3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) orf/io-xylene, by gas chromatography, test, D 3797 (06.03) purity analysis of isopropylbenzene (cumene), by gas chromatography, test, D 3760 (06.03) purity/benzene content of cyclohexane 995, by gas chromatog raphy, test, D 3054 (06.03) purity of aldehydes and ketones, test, D 2192 (06.03) purity of hydrocarbons from freezing points, test, D1016 (06.03) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography, test, D 3893 (06.03) purity of methyl ethyl ketone, using gas chromatography, test, D 2804 (06.03) purity of methyl isobutyl ketone, by gas chromatography, test, D 3329 (06.03) purity of propylene glycol monomethyl ether/'dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) purity of styrene, by freezing point method, test, D 3799 (06.03) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D'29 (06.02) sodium glycolate content of sodium carboxymethylcellulose, test, D 1439 (06,02) solidification point of4,4- isopropylidenediphenol (Bisphenol A), test, D 4493 (06.03) styrene, by gas chromatography, test, D 3962 (06.03) Pyridine aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03} hydroxyl content of cellulose acetate, by spectrophotometry, test, D 871 (06.02) hydroxyl content of pyridine-soluble cellulose esters, by spectrophotometry, test, A D 817 (06.02) pyridine base content in cresylic acid, by direct titration, test, D 4471 (06.03) sampling/handling liquid cyclic products (at amhient temperature), practice, D 3437 (06.03) water content, by iodine reagent method, test, D1631 (06.03), water content of paints/paint materials, by Karl Fischer method, test, D 4017 (06.01) Protective linings j|' design/fabrication of flue gas'd'esulfurization system components (for protective lining application), spec., D 46l8 (06.01) inspection of linings in operating flue gas desulfurization systems, practice, D 4619 (06.01) Pyridine--refined reducing substances ip, test, D 2031 (06.03) refined pyridine (1 decree), spec., D 2323 (06.03) water solubility, test, 6,2030 (06.03) Pyrolysis " 'russian blue <' See Iron blue full testing ... . field identification of coatings, test, D 5043 (06.01) Pyrophyllite See Magnesium silicate Sa -^Adhesion (headings) adhesion of organic coatings to.plastic substrates, by direct tensile testing, D 5179 (06.01) bond strength of thermoplastic traffic marking materials, using !> :: * cement bricks/steel cubes, test, D 4796 (06.01) pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) sfLSmethCfcfeJ3 i *a Pulp solubility in sodium hydroxide, test, D1696 (06.02) umice/pumice stone/pumacite :(fe.tfi>v' >.* t tfeif-KA,, pumice pigment, spec., D 867 (06.02) purity acetaldehyde, spec., D 4710 (06.03) personnel acrylate esters, by gas chromatography, test, D 3362 (06.03) alcohol content/purity of acetate esters, by gas chromatography, test. D 3545 (06.03) analysis ofp-xylene, by gas chromatography, method, Jayi " ^ S- PVO^t| Ifcftlti D 3798 (06.03) chemical analysis of benzene, by gas chromatography, test, D 4492 (06.03) ethyl methyl pentanol content/purity value of 2-ethyIhexanol, by gas chromatography, test, D 5008 (06.03) methyl acrylate, spec., D 4709 (06.03) Q Qualifications--nuclear facilities coating contractors (for nuclear-powered generation facilities), practice, D 4286 (06.01) establishing procedures to qualify/certify inspection personnel for coating work in nuclear facilities, guide, D 4537 (06.01) journeyman painters for application of coatings to concrete surfaces of safety-related areas in nuclear facilities, practice, D 4227 (06.01) journeyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities, practice, D 4228 (06.01) sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Qualification testing use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) Qualitative analysis/measurement white titanium pigments, chemical analysis, test, D1394 (06.02) Quality assurance coatings for light-water cooled nuclear power plants, practice, D3843 (06.01) 1179 DUP0502 98355 Quality assurance Index of ASTM Standards, Section 6 use of protective coating standards in nuclear power plants, selecting ASTM standards, guide, D 5144 (06.01) Quality control color of cresylic acids ("C" series standards), test, D 3627 (06.03) Quantitative analysis white linseed oil paints- chemical analysis, selecting test methods, practice, 0 215 (06.01) Quinoline water content, by iodine reagent method, test, D1631 (06.03) Radiation exposure accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, 0 4141 (06.01) effects of radiation on coatings (for light-water nuclear power plants); test, 04082 (06.01) exposure of paints/related coatings to fluorescent UV- condensation light-water-exposure apparatus, practice for conducting tests, 0 4587 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (06.01) ultraviolet-cured coatings, cure time, practice, 0 3732 (06.01) use ofprotective coating standards in nuclear power plants, selecting ASTM standards, guide, 0 5144 (06.01) Rapid deformation See Deformation (headings) Rare earths content paint driers, by EDTA method, test, D 3989 (06.03) Rate of evaporation , See Evaporation--rste/tiine Raw oils (drying oils) See Oils (headings) Raw sienna Sa Pigments (headings) chemical analysis of yellow/orange/red/Brown pigment's containing iron/maganese, test, D 50 (06.02) raw/burnt sienna pigments, spec., D'765 (06.02) Reactor vessels See Nuclear reactor vessels (headings) Reagent resistance factory-applied coatings on wood products, practice, D 3023 (06.01) Reagents presence of and removing microbial (fungal/algal) growth op paint/related. coatings, guide, D 4610 (06.01) Reagent water--microelectronic processing microelectronic device processing, spec., 01193 (06.03) Records management single-/mu!ti-panel forms for recording results of exposure tests of paints, A 01150 (06.01) Red copper oxide See Cuprous oxide Red iron oxide (hematite) See Iron oxide red Red oxide of mercury See Mercuric oxide Red pigments Sa Para (paranitraniline) rcd/ToiUidine red/Vehetian red chemical analysis of yellow/orange/red/brown pigments containing iron/magancse, test, D 50 (06.02) lead peroxide/true red lead content of dry red lead pigments, test, D 49 (06.02) natural red/brown iron oxide pigments, spec., D 3722 (06.02) para red/toiuidine red pigments, testing, 0 970 (96.02) pure para red toner pigment, spec., D 475 (06.02) pure toluidine red toner, spec., D 6S6 (06.02) red lead pigment, spec., D 83 (06.02) synthetic red iron oxide pigment, spec., D 3721 (06,02) Reduction refined pyridine, by reducing substances, qualitative determination, test, D 2031 (06.03) Redwood wood used as panels in weathering tests ofcoatings snec. 0 358(06.01) Referee methods total, primary, secondary, and tertiary amine values, of fatty amines, amidoanines, and diamines, test, D 2073 (06.03) Reference photographs chalking (of white/lightly tinted exterior paint films), practice AD 4214 (06.01) Refined benzene See Benzene (headings) Refined bleached lac See Bleached lac--dry Refined cresylic acid '.See Cresylic acid ' Refined naphtha derivatives See Naphtha and naphtha derivatives Refined phenol Sa Phenol refined phenol, spec., D 2439 (06.03) Refined phthalic anhydride See Phthalic anhydride , Refined pyridine,; . See Pyridine--refined Refined soybean oil See Soybean oil Refined tar acids See Tar acids--crude and refined Reflectance and reflectivity chalking (of white/lightly tinted exterior paint films), practice, AD4214 (06.01) gloss differences between surfaces of! similar appearance, method for visual evaluation, 0 4449 (06.01) gloss of high-gloss metallic/honmeiallic surfaces, by goniophotometry, method, E 430 (06.01) hiding power of paints, by reflectometry, test, A D 2805 (06-01) instrumental color difference, test, D 2244 (O6>01) porosity of paint films (to indicate coating penetration), test, 03258(06.01) '*7 reflection haze (of high gloss surfaces), test, D 4Q39 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) Reflectance and reflectivity--copy materials directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) preparation of reference white reflectance standards, practice, E 259 (06.01) Reflection haze See Haze Reflective markers in traffic paint See Glass spheres (in traffic paint) Refractive index gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) sampling and testing dipentene, method, D 801 (06.03) sampiing and testing pine oil, method, D 802 (Q6.03) sampling and testing turpentine, method, D 233 (06.03) Regular bleached lac See Bleached lac--dry Relative dry hiding power (of paints/coatings) See Hiding power--paints/coatings 1180 1, Rela R< re: DUP050298356 Index of ASTM Standards, Section 6 Resistance Relative humidity See Humidity--relative Relative fluting strength Sa Tinting strength > relative tinting strength of ptinting ink dispersions, test, D 2066 (06.01) Reporting point film failure See Failure end point (headings) Residual glycol ether purity of propylene glycol monomethyl ether/dipropylene glycol monomethyl ether/propylene glycol monomethyl ether acetate, test, D 4773 (06.03) Residual odor See Odor Residue chemical/gravimetric analysis of whitc/yellow thermoplastic traffic marking material containing lead chromate and < titanium dioxide, test, D 4797 (06.01) sampling/testing flaked aluminum powders/pastes, methods, D480 (06.03) Residue--evaporation naphthalene, test, D 2232 (06.03) sampling, end testing turpentine, method, D. 233 (06,03) Resiins alcohol-benzene soluble matter in cellulose, test, D 1794 (06.02) amine resins--solvent tolerance, test, D 1)915 (06.02) amino resins, selecting test procedure^,practice, D 4277 (06.02) clarity/cleapness of (nonpigjnented) paint and. ink liquids, by visual examination, test, 0 2090 (06.02,06.03) field identification of coatings, test, D 5043 (06.01) flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) , free formaldehyde content of amino resins, test, D 1979 (06.02) po!y(yinyl butyral> chemical analysis, test, D1396 (06.02) poiyCvinyl chidritie) resins, selecting test procedures, guide, D4368 (06.02) residuhl chloridg.Aonbmer content of poly(vinyl chloride) resins/compouhds/copolymers by solution injection technique, test, D 3680 (06.02) ! resin solution dilutability, test, D 5062 (06.03) ! softening point, by ring-and-ball apparatus; test, E 28 (06.03) solubility range, test, D 3132 (06.02) volatile/nonvolatile content (of cellulosics/emulsiofis/resin ; solutions/shellac/vamishes), selecting test procedures, practice, D 4209 (06.02) volatile resin acids in tall oii/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) , . water content of paints/paint materials, by Karl Fisoher method, test, D 4017 (06.01) , Resins--alkyd ,, artists' paints (oil/resm-oil/alkyo),;Spec., D 4302(06.01) fatty acids content, test, D 1398 (06.02) glycerol/ethylene glycol/pentaerythritol in alkyd resins, test,, . 01615 (06.02) identification of carboxylic acids in alkyd resinsjt> 2455 (06.02) identification of polyhydrit alcohols in alkyd resins, qualitative/quantitative analysis, test, D 2456 (06.02) isophthalic acid content of alkyd/polyester resins, test, D 2690 (06.02) phttialic anhydride content (in absence of dibasic acids), test, D 563 (06.02) phthalic anhydride content (in presence of dibasic acids), by gravimetric test, 01306 (06.02) polyhydric alcohols in alkyd resins, qualitative analysis, test, D2998 (06.02) rosin acids content, test, D1469 (06.02) silicone-modified-silicon content, by atomic absorption spectrophotometry, test, D 3733 (06.02) * specific gravity at 25/25"C, test, D1963 (06.03) testing, practices, I> 2689 (06.02) unsaponifiable matter content, test, D 1397 (06.02) Resins--epoxy bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test; D4796 (06.01) epoxy content of epoxy resins, test, D 1652 (06.02) epoxy resins, selecting test procedures, practice, D 4142 (06.02) hydrolyzable chlorine content of liquid epoxy resins; test, D 1726 (06.02) nitrogen (total) content of nitrogen-containing plastics/ resihs/resin solutions, test, D1013 (06.02) total chlorine content in epoxy resins/compounds, test, D4301 (06.02) total chlorine content, test, D1847 (06.02) Resins--lac ' orange shellac/other indian lacs for electrical insulation, spec., D 784 (06.02) sampling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, 029 (06.02) Resins--nitrogen amino resins, selecting test procedures, practice, 0 4277 (06;02) nitrogen (total) content of nitrogen-containing plastics/ ' resins/resin solutions, test, D 1013 (06.02) Resins--phenolic apparent free .phenols, jn-synthetic phenolic resins/solutions (used"in paints/related coatings), test, D1312 (06.02) apparent pH of water insoluble phenol-formaldehyde resin, test, D 4613 (06.02) methylol group determination (qualitative) in phenolic resins, test, 0 4706(06.02) stroke cure time of thermosetting phenol-formaldehyde resins, test, 0 4640 (06.02) volatile content in phenolic resins, test, D 4639 (06.02) Resins--resin solutions laboratory preparation of gelled vehicles, using microwave oven, practice, 05166 (06.02) Resin solution cloud point resin solution dilutability, test, D 5062 (06.03) Resin solutions color of transparent liquids, by Gardner color scale, test, D 1544 (06.01,06112, 06.03) glycerol/ethylene glycol/pentaerythritol in alkyd resins) test, D 1615 (06.02) nitrogen (total) content of nitrogen-containing plastics/ resins/resiri solutions, test, D 1013 (06.02) nonvolatile content of printing inks/resin solutions/vehicles, test, D4713 (06.01) nonvolatile content of resin solutions (in volatile organic solvents), test, 0 1259 (06.02) . . . .. . phthalic anhydride content, in absence ofdibasic acids, test, 0 503 (06.02) - resin solution dilutability, test, D'5062 (061)3) unsaponifiable matter poptent, test, D1397 (06.02) viscosity, test, D1725 (06.02) Resistance See Resistance--abrasion Sa Resistance--acid Resistance--alcohol Resistance---alkali Resistance--bacteria Resistance--blistering Resistance--blocking Resistance--chemical Resistance--chipping Resistance--cracking Resistance--deformation Resistance--fuel Resistance--heat Resistance--impact (pipeline coatings) Resistance--imprinting Resistance--mortar Resistance--oil Resistance--paint spatter 1181 DUP050298357 Index of ASTM Standards, Section 6 Resistance--penetration Resistance*--pressure mottling Resistance--reagent Resistance--sag Resistance--scrub Resistance---slip Resistance--solvent Resistance--temperature : Resistance--water Resistance--abrasion (paints/related coatings) abrasion resistance of organic coatings, by falling abrasive, test, D 968 (06.01) , abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, D 5181 (06.01) air blast abrasion tester, A D 6S8 (06.01) practical washability of organic coatings, test, D 4828 (06.01) resistance of steel pipeline coatings to abrasion, by.slurry of coarse abrasive/water, test, G6 (06.01) Taber abraser, test, D 4060 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) Resistance--acid acid/mortar resistance of factory-applied clear coatings on extruded aluminum products, test, D 3260 (06.01) Resistance--alcohol wood furniture lacquers, test, D 2571 (06.01) Resistance--alkali clear/pigmented organic coatings, test, D1308 (06.01) dried varnish films, test, 01647 (06.01) Resistance--bacteria resistance of emulsion' paints (in containers) to attack by microorganisms, test, D2574 (06.01) resistance to mold growth on surface of interior paint coatings (in an environmental chamber), test, D 3273 (06.01) , Resistance--blistering , evaluating degree of blistering, method, A D 714 (06.01) testing water resistance of coatings, using controlled condensation, practice, D 4585 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D 1735 (06.01) Resistance--blocking blocking resistance of trade sales paints, test, D 4946 (06.01) organic coatings on wood substrates, test, D 2793 (06.01) pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06.01) Resistance--boiling water (H20) wood furniture lacquers, test, D 2571 (06.01) Resistance--chemical chemical resistance of pipeline coatings, test, G 20 (06.01) clear/pigmented organic coatings, test, D1308 (06.01) coatings for light-water cooled nuclear power plants, D 3912 (06.01) Resistance--chipping paints and related coatings, A D 3170 (06.01) traffic paint, A D 913 (06.01) Resistance--coffee stain wood furniture lacquers, test, D 2571 (06.01) " Resistance--corrosion See Corrosion (headings) Resistance--cracking See Cracking--coatings Resistance--deformation penetration resistance of pipeline coatings, by blunt rod test, G17 (06.01) resistance of organic coatings to effects of rapid deformation (impact), test, D 2794 (06.01) Resistance--detergent organic finishes, practice, D 2248 (06.01) Resistance--fiiel solvent/fuel resistance of traffic paint, test, D 2792 (06.01) Resistance--heat evaluating (interior/exterior) coatings for rrowotKp steel surfaces at high-temperature sernce test, a D2485 (Oh III i temperature-change (high-low) resistance ot'cle, ', lacquer films applied to wood, test,; 121] ((}(,.{} I) Resistance--imprinting print resistance of architectural painls, test, D 2064 (06,1)1) print resistance of lacquers, test, D 2091 (06.(11 Resistance--mar mar resistance of orgaaic coatings, using balanc.i o. n i scran adhesion and mar test, D 5178 (06.01) Resistance--mortar acid/mortar resistance of factory-applied clear couvies on extruded aluminum products, test, D3260 (06 01) Resistance--oil wood furniture lacquers, test, D 2571 (06.01) Resistance--paint spatter paint spatter resistance to roller application, test; D 4"ir nn, m, Resistance--penetration porosity of paint films (to indicate coating penetrationi test D 3258 (06.01) Resistance--pipeline coatings, cathodic disbonding of pipeline coatings, accelerated procedure test, G 8 (06.01) comparative corrosion preventive characteristics of materials used.fbf joints/couplings/fittiftgs/patches in pipeline' ' coatings, test, G18 (06.01) ' ' ' ` effects of outdoor weathering on pipeline coatings, test, Gil (06.81) impact resistance of pipeline coatings, by falling weight test, G 14 (06.01) impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) specific bendability of pipeline coatings, test, G10 (06.01) Resistance--pressure mottling pressure mottling/blocking resistance of organic coatings (on metal substrates), test, D 3003 (06.01) Resistance--reagent factory-applied coatings on wood products, practice, D 3023 (06.01) Resistance--sag sag resistance of paints, using a multinotch applicator, test, D 4400 (06.01) Resistance--scrub scrub-to-failure of interior latex flat wall paints, test/ D 2486 (06.01) wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D4213 (06.01) Resistance--slip static friction ofcoating surfaces, test, D 4518 (06.01) Resistance--soil practical washability of organic coatings, test, D 4828 (06.01) Resistance--solvent solvent/fuel resistance of traffic paint, test, b 2792 (06.(il) Resistance--stain factory-applied coatings on wood products, practice, D 3023 (06.01) practical washability of organic coatings, test, D 4828 (06.01) Resistance--temperature temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D1211 (06.01) Resistance--water coatings using controlled condensation, practice, D 4585 (06.01) coatings, using water immersion, practice, D870 (06.01) dried varnish films, test, D 1647 (06.01) testing water resistance of coatings at 100 % relative humidity, practice, D 2247 (06.01) testing water resistance of coatings, using water fog apparatus, practice, D 1735 (06.01) vF 1182 Resistan S& Resistan praoti Retort i St Retrore sieve Rheolo; print Rheoloi rheol statii Rich gi Rolle pie pai Rolle Hie -Ro|I< Rose io<RosiL akf am in oA Si ft: DUP050298358 Index of ASTM Standards, Section 6 Resistance--wear See Wear testing (headings) Resistance--wet abrasion practical washability of organic coatings, test, D4828 (06.01) Retort pine tars See Pine tars (kiln and retort) Retroreflection/retroreflectors sieve analysis of glass spheres (for retroreflective pavements maridngs/industrial uses), test, D 1214 (06.02) Rheology printing inks/ink films/related materials, selecting test methods, guide, D 5010 (06.01) Rheology/rheological properties rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) static friction of coating surfaces, test, D 4518 (06.01) Rich gold bronze powder See Copper powder ' Sa Gold bronze powder Ring-and-ball apparatus softening point test of resins, E 28 (06.03) Rivets paint films, evaluating degree of surface disfigurement, AD3274 (06.01) Road service testing . Sa Traffic'paint conducting road service tests on fluid traffic marking materials, practice, D 713 (06.01) evaluating degree of bleeding of traffic/pavement marking paint, test, A'D 868 (06.01) evaluating degree ofchipping of traffic paint, method, A D 913 (06>01) Rocker hardness test (Sward) See Hardness tests--Sward (rocker) Roller preparation of paint roller covers for evaluation, D 5069 (06.01) Roller application paint spatter resistance to roller application, test, D 4707 (06.01) Roller application of paints hiding power of architectural paints applied by roller, test, D 5150 (06.01) Roller coat testing industrial water-reducible coatings, guide, D4712 (06.01) Rosenmund-Euhnhenn method iodine value of drying oils and their derivatives, test, D1541 (06.03) Rosin acid number, test, D 465 (Q6.03) ash content, after burning hnd ignition, test, D1063 (06.03) iron content, test, D1064 (06.03) oleic acid content of tall oil rosin, test, D1585 (06.03) sampling/grading rosin (delivered in commercial bags/ barrels/drums), test, D 509 (06.03) saponification number, test, D 464 (063)3) unsaponifiable matter content, test, D 1065 (06.03) volatile oil in rosin, test, D 889 (06.03) volatile resin acids in tall oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) Rosin acids content coating vehicles (rosin esters, varnishes, and alkyd resins), test, D1469 (06.02) fatty acids, test, D 1240 (06.03) rosin oils, testing, D 1131 (06.03) sampling/testing lac resins (orange shellac/button lac/garnet lac/bleaChed lac), test, D 29 (063)2) tall oil, methods of testing, D 803 (06.03) Rosin content qualitative detection of rosin in varnishes, by LiebermanStorch/Halphen-Hicks tests, D 1542 (06.01, 06.02) Sampling--hydrocarbons Rosin esters rosin acids content, test, D 1469 (06.02) Rotational viscometer rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) Rouge See Iron oxide red Roundness of glass spheres embedded in traffic paint, test for, D 1155 (06.02) Rubber--general mandrel bend test'of attached organic coatings, test, D 522 (06.01) Rub-out test absorption of linseed oil in pigments, test, D 281 (06.02) Rupture/rupture strength impact resistance of pipeline coatings, by falling weight test, G14 (06.01) impact resistance of pipeline coatings, by limestone drop test, G13 (06.01) Rust degree of rusting on painted steel surfaces, method, AD 610 (06.01) Rust breakthrough assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) Rutile ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, D 3720 (06.02) s Safety precautions--coating applications design/use of safety alert system for.hazard.ous work locations in coating/lining industry, practice, A D 4257 (06.01) establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, D 5163 (06.01) handling naphthalene, maleic/phthalic anhydride, practice, D 3438 (06.03) handling phenol and cresvlic acid, practice, D3852 (06.03) handling polymeric powders, practices, D 3451 (06.01) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) Safflower oil safflower oil, spec., D1392 (06.03) Sag resistance paints, using a multinotch applicator, test, D 4400 (06.01) Salt water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) Salt spray (fog) testing salt spray (fog) testing, method, B 117 (06.01) Sample preparation sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) Sampling industrial chemicals, practice, E 300 (06.03) Sampling--aerospace fluids lead/chromium content (in air particulate filter samples of lead chromate type pigment dusts), by atomic absorption spectroscopy, test, D 4358 (06.02) Sampling--hydrocarbons cresylic acid and phenol, practice, D3852 (06.03) naphthalene, maleic anhydride, and phthalic anhydride, practice, D 3438 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling 4,4- isopropyiidene diphenol (bisphenol-A), practice, D 4297 (06.03) 1183 DU PO 502 98359 Sampling--hydrocarbons Index of ASTM Standards, Section 6 sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) Sampling--paints/related coatings industrial chemicals, practice. E 300 (06.03) paints/pigmented coatings (from containers), practice, D 3923(06.01) sample preparation for qualification testing of coatings (used in nuclear power facilities), spec., D 5139 (06.01) sampling and testing shellac varnish, D1650 (06.02) sampling and testing turpentine, method, D 233 (06.03) sampling/grading rosin (delivered in commercial bags/ barrels/druths), test, D 509 (06.03) sampling liquid oils/fatty acids (commonly used in paints/ varnishes/related materials), test, D1466 (06.03) sampling/testing high-gravity glycerin, test, D1258 (06.03) sampling/testing lac resins (orange shellac/button lac/gamet . lac/bleached lac), test, D 29 (06.02) sampling/testing pine tars/pine-tar oils, test, D 856 (06.03) sampling/testing volatile solvents/chemicai intermediates (for paints/iacquer/vamish/reiated material), selecting test methods, D 268 (06.03) Sampling--petroleum products purity of hydrocarbons from freezing points, test, D1016 (06.03) Sand i abrasion resistance of organic coatings, by falling abrasive, test, D 968 (06.01) Sandstone preparatory surface cleaning of architectural sandstqne, practice, D 5107 (06.01) Saponification nutnber/vaiue Sa Unsaponifiable matter content apparent acetyl content of cellulose acetate proprionate/ butyrate, test, A D 817 (06.02) rosin, test, D 464 (06.03) samplingand testing Shellac varnish, D1650 (06.02) ` sampling/testing- lac resins (orange shellah/button lac/gamet lac/bleached lac), test, D 29 (06.02) saponification value of drying oils/fatty acids/polymerized' fatty acids, test, D1962 (06.03) tall oil, methods of testing, D 803 (06.03) Saybott viscometers See Viscometers--Sayboit Scaling " See Flaking Scattering coefficient hiding power of paints* by refiectometfy, test, A D 2805 (06.01) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) Scrub resistance , scrub-to-failure ofinterior latex flat.wall paints, test, D 2486 (06.01) Sealers (floor) See Floor paints/coatings Secondary butyl acetate (85-88 % grade) See -Butyl acetate (all grades) Secondary butyl alcohol See sec-Butyl alcohol Sediment clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) Sedimentation reporting particle size characteristics of pigments, practice, D1366 (06.02) Self-aligning adhesion tester pull-off strength of coatings, using portable adhesion testers, test, D 4541 (06.01) Semi-gloss paints interior latex semigloss/gloss paints, selecting test methods, guide, D 4540 (06.01) Sensory evaluation--odor x, > ^ volatile solvents and diluents, test, D1296<.06.03) " Sendee Level I establishing procedures to monitor perfortnance.o: safeu lolMed" coatings in operating nuclear power phm cuuh , " ', 05163(06111) , Service level I and II use of protective coating standards in nircle-u power plants selecting ASTM-standards, guide, DS144 ,06.01) Setaflash testers flash point of liquids, by Setaflash closed-cup ann irutus tv D 3278 (06.03) ,' sustained burning (of liquid mixtures), by Seta-flash tester (oiertcup), test, D 4206 (06.01,06.03) Settlement evaluating degree- of settling (pigment suspension/case of remixing a shelf-aged sample) of paint, leu, DSh'J (llb.lll) . traffic paint, in containers, by laboratory sii nidation test D1309 (06.01) Set-to-touch-time See Drying time Shear testing--paints/relpted coatings/materials consistency of paints, using Stormer viscometer, test, D 562 (06.01) subjecting marine antifouling coating to bifoulipg and fluid shear forces in natural seawater, test, D4939 (06.01) viscosity of printing inks/vehicles, by falling-rod viscometer,, test, D 4040 (06.01) Shear thinning - r > . - -- ; . ..... rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) Sheen 1 Sa Gloss ,, gloss/sheen uniformity evaluation, test, D 3928!(06j01) . practical washability of organic coatings, test, D 4828 (06.01):, specular gloss of nonmetallic. specimens, test, D 523 (06,01) Sheet materials (general) continuity verification of liquid/sheet linings applied to concrete substrates, practice, D4787 (06.01) .... ./fji Sheet metal flexibility/adhesion of organic coatings (paints) on prepainted deformed metallic sheets, test, 04145(06.01) , mandrel bend test .of attached organic coatings, test, !jfy D522 (06.01) ' Shellac - ...... samplingand testing shellac varnish, D1650 (06.02) shellac varnishes, spec., D 360 (06.02) volatile/nonvolatile content (ofceHulosics/emulsions/resin fl solutions/shellac/varnishes), selecting test procedures, practice, D 4209 (06.02) ' Shellac--electrical insulating ,, ... ; orange shellac/otber Indian lacs for electrical insulation, spec.,, D 784 (06.02) shellac (dry/powdered) qsed for electrical insulation, selecting test methods, D 411 (06,02) Shellac--orange dt Orange shellac and (button lae/garnet lac),, spec., D 237 (06.02) sampling and testing shellac Varnish, D 1650 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, D 29 (06.02) Shipping amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) impact resistance of pipeline coatings, by falling weight test, G14 (06.01) Shortness ratio laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) 1184 ill U-tit: DUP050298360 Lnde\ G AS I'M Siandardi*Section^ Solid pI<.<G* in.itcri.i1s -- p inns riliiul v minus materials Short-radius bends specific bendability of pipeline coatings, test, G 10 (0&01) SI (International System of Units) use of international system of units (SI) (modernized metric system), excerpts, (Related Material--all volumes) (06.01,06.02,06.03) Sienna (burnt and raw) chemical analysis of yeUow/orange/red/brown pigments containing iron/maganese, test, D 50 (06.02) raw/bumt sienna pigments, spec., D 765 (06.02) Sieve analysis sieve analysis of glass spheres (for retroreflective pavements markings/industriai uses), test, D 1214 (06.02) Sieve analysis--subsieve reporting particle size characteristics of pigments, practice, D1366 (06.02) Silanes/Siloxane nonvolatile content in silanes/siloxanes/sfiane-siloxane blends used in masonry water-repellent treatments, test, D 5095 (06.01) Silica content acid-soluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, 01135 (06.02) cellulose, test, 0 2438 (06.02) chromium trioxide content of basic lead silico-chromate pigment, test, 01844 (06.02) free silica in barium sulfate pigment, test, 0 715 (06,02) white titanium pigments, chemical analysis, test, 01394 (06.02) Silica (diatomaceaus) diatomaceous silica pigment, spec., D 604 (06.02) Silicon content silicon polymers and silicon-modified alkyds, by atomic absorption spectrophotometry test, 0 3733 (06.02) Silicon dioxide (Si02) content silicon dioxide in magnesium silicate pigment, test, D 717 (06.02) ' Silicone-coated paper preparation of free films of organic coatings, practice,, D 4708 (06.01) Silicone-modified alkyds silicon content, by atomic absorption spectrophotometry, test, D 3733 (06.02) Silicone polymers silicon content, by atomic absorption spectrophotometry, test, D 3733 (06.02) Simulated accident conditions purity of methyl isobutyl ketone, by gas chromatography, test, D 3911 (06.01) Single-panel forms recording results on single-/multi-panel forms, method, A D 1150 (06.01) Skinning See Stability--trackage Skins content clarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) S!ag . . conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, D 4940 (06.01) Sliding scale calibration graph viscosity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) Slip resistance static friction of coating surfaces, test, D 4518 (06.01) Slope laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) Slump slump of face glazing/bedding compounds on metal sash, test, D 2376 (06.01) Slurries ,,nnJucumeti it analysis o'wa.-ei-'-oluhle lop.c contamination of oUiStrngiabidMres, tcsi D 4940 (06.01) resistance ot steel pipeline cnalincs to abrasion by'Stirry of coaie abrustveAvate* test, G 6 (06.01) weight percent il >It us m aqueous s.uu c, of titanium dioxide pigments, test, D 3026 (116,02) Smudging 1> abrasion resistance of printed matter, by the ga-cat comprehen sive abrasion test, 05181 (06.01) Soapstone See Magnesium silicate '` Sodium carboxymethylcellulose sodium glycolate content of sodium carboxymethylcellulose, test, D1439 (06.02) Sodium glycolate content sodium glycolate content of sodium carboxymethylcellulose, test, D1439 (06.02) Sodium hydroxide (caustic soda) residual p-tert-butyicatechol (TBQ in styrene monomer, by addition of NaOH, test, 0 4590 (06.03) solubility in sodium hydroxide, test, 0 1696 (06.02) Sodium sulfite ,, free formaldehyde content of amino resins, test, 01979 (06.02) Softening point clear/pigmented organic coatings, test, 0 1308 (06.01) resins, by ring-and-ball apparatus, test, E 28 (06.03) Soil accumulation paint films, evaluating degree of surface disfigurement, A 0 3274 (06.01) Soil burial test disbonding characteristics of pipeline coatings, by direct soil burial, test, G19 (06.01) Soil removal properties practical washability of organic coatings, test, 0 4828 (06.01) Solar spectral irradiance operating light-exposure .apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Solidification point 4,4- isopropylidenediphenol (Bisphenol A), test, 0 4493 (06.03) aromatic hydrocarbons/related chemicals, terminology, D 4790 (06.03) benzene, test, 0 852 (06.03) solidification point of industrial organic chemicals, test, 0 1493(06.03) solidification (titer) point of fatty acids, test, 01982 (06.03) Solid phase materials--paints/related coatings/matcrials amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, 0 4948 (06.01) calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) determining liquid/solid status (of viscous materials), test, 0 4359(06.01) filter-retained solids content of polymer latexes, test, O 5097 (06.02) flash point (of fuel oils/lubc oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, D 2621 (06.01) toluene-insoluble solid matter (sand/chips/dirt/bark) in rosin, test, 0 269 (06.03) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/vamishes), selecting test procedures, practice, D 4209 (06.02) volatile/nonvolatile content (of driers/drying oils/naval stores and solvents), selecting test procedures, guide, D 4140 (06.03) 1185 DUPO 502 98361 Index of ASTM Standards, Section 6 Solidphasematerials- -paints/related coadngs/materials volatile/nonvolatile content (of pigments), selecting test procedures, guide, D4139 (06.02) . weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D 3926 (06.02) infrared identification of vehicle solids from sohcm-iedu-'iblc paints, by infrared spectroscopy, test, 1) 2021 (06.01) interior flat wall paint, selection/use of test methods, iiracd... D 3323 (06.01) ' Solubility interior semigloss waUArim enamels, selection/use of test refined pyridine in water, test, D 2030 (06.03) `methods, practice, D 3425 (06.01) ' resin solution dilutability, test, D 5962 (06.03) solubility in sodium hydroxide, test, D1696 (06.02) lead/cadmium/cobalt content (low concentrations) in nonvolatile-portion of liquid coatings/dried films, by solubility range (of resins/polymers),, test, D 3132 (06.02) soluble cellulose nitrate, testing, methods, D 301 (06.02) atomic absorption spectroscopy, test, D3335 (06-.01) lead content in paint; by direct aspiration atomic absorption Solubility--alkali spectroscopy, test, D 4834 (06.01) solubility in sodium hydroxide, test, D 1696 (06.02) mandrel bend test of attached organic coatings, test Soluble cellulose nitrate nitrocellulose D 522 (06101) soluble cellulose nitrate, testing, methods, D 301 (06.02) mercury content (low concentrations) in liquid COatings/poatmgk Soluble sulfates content vehicles/dried films, by atomic absorption spectroscopy " .a lead peroxideArue red lead content of dry red lead pigments, , test, D 49 (06.02) test, D 3624 (06.01) i nature of thinners in solvent-reducible paints, qualitative Solution injection technique determination, method, D2349 (06.01) residual vinyl chloride monomer content of polyfvinyl chloride) resins/compounds/copolymers ,by solution injection package stability of solvent-reducible/water-reducible paint test D 1849 (06.01) ' technique, test, D 3680 (06.02) , paint spatter resistance to roller application, test D 4707 (06.01)' Solvent analysis (of solvent-type paints) , direct injection with a gas chromatograph, practice, pigment Content, high-speed: centrifuging, test; D 2698 (06.01): pigment content Of solvent-reducible paints, test, D 2371 (06.01) D. 3271 (06.01) Solvent and fuel resistance of traffic paints See Traffic paint porosity of paint films (to indicate doatihg penetration), test: 0 3258(06.01) ': ' practical washability of organic coatings, test, D 4828 (06(01) Solvent brushing and wiping , Sa Steel panels preparation of hot-dipped nonpassivated galyanized steel,panels for testing paint/varnish/lacquer/relatbd products, test,' D 2201 (06.01) Solvent-extractable matter pigment content of solvent-reducible paints, test, D 2'371{06.01) Solvent naphtha (refined) See Naphtha and naphtha derivatives ' Solvent-reducible paints/coatings amount of liquid separated as upper layer from a viscous solution/dispersion containing dispersed 'solids, test, D 4948 (06.01) antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3717 (06.01) antimony oxide content of white pigment (separated from solvent-type paints), test, D 2350 (06.02) artists' paints (oil/resin-oil/alkyd), spec., D4302 (06.01) blocking resistance of trade sales paints; test, D 4946 (06.01) calculating formulation physical constants of paints/cdatings, . practice,'D 5201 (06.01) " chrdmium content (low concentrations) in solids of liquid preparing drawdowns-of artiits'paste paiits, practice' D4941 (06.01) 1? relative tinting strength of chromatic paints, tesi;l> <181(8 (06.01)' solvent analysis, by ggk chromatography direct injection method, practice, 03271(06.01) subjecting marine ahtiftwling coating to bifouling and fluid shear forces in natural seawater, tdst, D 4939 (06.01) sulfide in white pigment separated fr&tn solyeht-rediicibte ' ' paints, test, O 2351 (06.02) sulfur dioxide in white pigment separated from solvent- reducible paints, test, D 2352 (06.02) testing solvent-borne architectural (interior/exterior) cdatiUgh, ' ' guide, D 5146 (06.01) ;, testing water resistance of coatings at 100; %:rdatite humidity, practice, D 2247 (06.01) titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D4764 (06.01) ' vacuum distillation (fdr vehicle separation in solvent-type paints), practice, D 3272 (06.01) vehicle separation from solvent-reducible paints, by centrifqge, practice,!) 2372 (06.01) volatile matter content determination, test, 1) 2369 (06,01) volatile organic compounds (VOCJoFsolvent reducible paints coatings/dried films, by atomic absorption spectroscopy, in aerosol cans, test, 155200 (06.01) test, D 3718 (06.01) volume nonvolatile matter in clear/pigmented coatings, test, commercial hexanes, spec., D 1836 (06.02) , . D 2697 (06.01) conducting tests on paint/vamish/Iacquer/related products, water content of paints/paint materials, by Karl Fischer using enclosed carbon-arc light/water exposure apparatus, method, test, D 4017 (06.01) practice, D 5031 (06,01) a) wet-to-dry hiding change of architectural coatings, test, directional reflectance factor (45-deg 0-deg) of opaque D 5007 (06.01) specimens, by broad-band filter reflectometry, test, wood used as panels in weathering tests of coatings, spec., E 97 (06.01) ' D 358 (06.01) erosion testing of antifouling paints, using high velocity water, test, D 4938 (06.01) exterior house/trim paint, selection/use of test methods, < practice, D 2932 (06.01) field identification of coatings, test, D5043 (06.01) floor paint, selection/use of test methods, practice, D 3383(06.01) hiding power of architectural paints applied by roller, test, D 5150 (06.01) Solvent release amount of volatile organic compound (VOC) released from solventborne automotive coatings and available for removal in a VOC control device (abatement), test, D 5087 (06.01) ; Solvent rub method MEK resistance of ethyl silicate (inorganic) zinc-rich primers, . by solvent rub, test, D 4752 (06.01) hiding power of paints, by reflectometry, test, A D 2805 (06.01) Solvents identification of oils and oil acids in solvent-reducible paints, field identification of coatings, test, D 5043 (06.01) test 02245(06.03) hexyl acetate, spec., D 5137 (06.03) 1186 trac Solve: > ani bei 1;, DUP050298362 Index of ASTM Standards. Section 6 Specimen preparation (for testing)--paints/related coatings mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., 0235(06.03) trace peroxides (2:5-80 ppm); using spectrophotometer, tests i F.299`(U6.03) Solvents--hydrocarbon aniline point/mixed aniline point of petroleum products/ hydrocarbon solvents, te&, D 611 (06.03) benzene content in hydrocarbon solvents;'by gas chromatog raphy, test, D4367 (06.03) Kauri-butanol value, test, D1133 (06.03) Solvents--paints/related coatings/materials acetone, spec., D 329 (06.03) acidity in volatile solvents/chemical intermediates (used in paint/varnish/lacquer/related products), test,:.!. D1613 (06.03) amount of volatile organic compound (VOG) released from solventbome automotive coatings and available for, ; removal in a VOC control device (abatement), test, D 5087 (06.01) n-butyl acetate (all grades), spec., D 4615 (06.03) calculating formulation physical constant%pf paints/coatings, practise, D 5201 (06.0J) ciarity/cleanness of (nonpigmented) paint and ink liquids, by visual examination, test, D 2090 (06.02, 06.03) commercial hexanes, spec., D1836 (06.03) . dichlorometiiane/l,l,i:trichloroetharie content in paints/ coatings, by direct injection gas chromatography, test, D4457(06.oi) , \ ester value of solvents'and 'tfiiiinets; test, 01617 (06.03) ethylacetate (all grades). spec,, D 4614 (06.03) ` heptahe miscibility Of lacquer solvents, test, D 1476 (06.03) hexyl acetate, spec., P 5137 (06.03) ispbutyl acetate (95 % grade), spec,, D1718 (06.03) methyl isobutyl ketone, spec., D 1153 (Q6.03) , ' mineral (petroleum) spirits hydrocarbon drycleanin'g solvent, spec., 0 235 (06.03) - ,, noriVolatife content of printing inks/resin soiutions/vehicles, test, D 4713 (06.01) ! nonvolatile content of resin solutions (in volatile organic- solventsL (est, D 1259 (06.02) nonvolatile'matter content, test, D1353 (06.03). -propyl acetate (96 % grade), spec., D 3130 (06.03) odor (charUcteristic/residual), test/D 1296 (06,03) ,, primary (synthetic) amyi acetate (98 % grade), spec., D3540 (06.03) purity of methyl (amyl ketone/isoamyl ketone), by gas chromatography,, test, D 3893(06.03) . , _ satnpling arid testing dipentene, method, D 801 (06.03) sampling/testing volatile solvents/chemical intermediates (for . paints/lfcquer/vamish/related material)', selecting test methods, D 268 (06.03) solvent composition analysis (in sulxent-typc 'paints),, by gas chromatography, test, D 3271 (06.01) , " solvent extractable material in black pigrhents, test, D 305 (06.02) solvent/fuel resistance of traffic paint, test, D 2792 (06.01) solvent tolerance, of amine resins, test, D1198 (06102) trace peroxides (>5-80 ppm), using spectrophotometer, test, E 299 (06.03) voiatile/non'volatile content (of driers/drying oils/naval stores and solvents), selecting'trist procedures, guide,D 4140 (06.03) water content of paints/paint materials, by Karl Fischer method, test, D 4017 (06.01) water in'volatile solvents, by-Fischer reagent titration method, test, 1) 1364(06.03) water miscibility of water-soluble solvents, test, D 1722 (06.03) Solvent tolerance resin solution dilutability, test, D 5062 (06103) Southern pine wood used as panels in weathering tests of coatings, spec,, 0 358(06.01) Soybeanoil degummed soybean oil, spec., D 124 (06.03) refined soybean oil, spec., 0 1462 (06.03) Spark-source mass spectrometry ` Sa Spectrophotometry (headings) color of cresyhc acids ("C" series standards), test, D 3627 (06.03) Spark testers discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D 5162 (06.01) Spattering paint spatter resistance to roller application, test, D 4707 (06.01) Spat test (for lead) detection of lead in paint/dried paint films, test, D 3618 (06.01) Spatula rub-out test absorption of linseed oil in pigments, test, D 281 (06.02) Specifications--petroleum 2-methoxyethanol, spec., D3128 (06.03) mineral (petroleum) spirits hydrocarbon drycleaning solvent, spec., D 235*(06.03) - Specifications--petroleum products commercial hexanes, spec., D1836 (06.03) Specific gravity--paints/related coatings/materials commercial density (of pure liquid chemicals), test, D 3505 (06.03) drying oils, varnishes, alkyd resins, fatty acids, and related materials, at 25/25G, test, D1963 (06.03) pigments, tests, D 153 (06.02) sampling.and testing dipentene, method, D 801 (06.03) sampling and testing pine oil, method, D 802 (06.03) sampling and testing pine tars/pine-tar oils, method, D 856 (06.03) . sampling and testing turpentine, method, D 233 (06.03) Specific permeability moisture vapor transmission of organic coating fdms, test, D 1653 (06.01) Specific resistance (resistivity)' water-soluble salts in pigments, by measuring specific resistance of pigment leachate, test, D 2448 (06.02) Specimen preparation (for testing)--paints/related coatings abrading concrete, practice, b 4259 (06.01) acid etching concrete, practice, D 4260 (06.01) magnesium alloys, practice, D 1732 (06.01) making and preparing coUcrete/masohry panels for testing paint finishes, method, D 1734 (06.01) paint and related coatings eXposure tests, methods for preparation, D 609 (06.01) pH of chemically cleaned/etched concrete surfaces, D 4262 (06.01) preparation of aluminum/aluminum-alloy surfaces (for painting), practice, D1730 (06.01) preparation of hot-dip aluminum surfaces (for painting), practice, D1731 (06.01) preparation of hot-dipped nonpassivated galvanized steel panels for testing paint/varnish/lacquer/related products, test, 0 2201 (06.01) preparation of methyl esters from fatty acids, for fatty acid composition analysis, test, D 3457 (06.03) preparation of paint brushes for-evaluation, practice, D 5068 (06.01) preparation of paint roller covers for evaluation, D 5069 (06.01) preparing drawdowns of artists' paste paints, practice, 0 4941(06.01) preparing glass panels for testing, D 3891 (06.01) reference White reflectance standards, practice, E 259 (06.01) selection of coating specimens and preparation for appearance measurement, practice, 0 3964 (06.01) 1187 Isiffll DUP050298363 Index of ASTM Standards, Section 6 Specimen preparation (for testing)--paints/related coatings standard pictorial surface preparation standards for painting steel surfaces, A D 2200 (06.01) surface cleaning concrete (for coating), practice, D 4258 (06.01) surface cleaning concrete unit masonry (for coating), practice, D 4261 (06.01) zinc-coated (galvanized) steel, practice, D 2092 (06,01) Specimen preparation (general)--paints/related coatings sample preparation for qualification testing of coatings (Used in nuclear power facilities), spec., D 5139 (06.01) Spectral data conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) directional reflectance factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, E 97 (06.01) gloss of high-gloss metajlic/nonmetallic surfaces, by goniophotometry, method, E 430 (06.01) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, ' practice, G 26 (06.01) Spectrometry--mass color of cresylic acids ("C" series Standards), test, D 3627 (06.03) Spectrophotometry--absorption carbon disulfide content of aromatic hydrocarbons, using spectrophotometry, test, D 2324 (06.03) iron content (of rosin), D 1064 (06.03) spectrophotometric diene value of dehydrated castor oil/derivatives, test, D1358 (06.03) thiophene content of benzene, by spectrophotometry, test, D 1685 (06.03) Spectrophotometry--atomic absorption (of paints/related coatings) lead content in paint, by direct aspiration atomic absorption spectroscopy, test,D 4834 (06.01) metals (iron/copper/manganese/calcium) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry, test, D 4085 (06.02) organotin release rates of antifouling coating systems in sea water, using graphite furnace atomic absorption spectrophotometry (GF-AAS), test, D 5108 (06.01) relative tinting strength of printing ink dispersions,,test, D 2066 (06.01) Spectrophotometry--goniophotometry gloss of high-gloss mctallic/nonmetallic surfaces, by goniophoto metry, method, K 430 (06.01) Spectrophotometry--infrared cellulose nitrate in alkyd lacquers, quantitative determination by infrared spectrophotometry, test, D 3133 (06.01) infrared identification of vehicle solids from solvent-reducible paints, by infrared spectroscopy, test, D-2621 (06.01) qualitative identification ofpolymers in emulsion paints, by infrared analysis/pyrolysis-gas liquid chromatography, practice, D 3168 (06.0,1) uniformity (of traffic paint vehicle solids), practice, D 2743 (06.01) Spectroscopy--absorption (of paint) lead/chromium content (in air particulate filter samples,oflead chromate type pigment dusts), test, D 4358 (06.02) lead content in paint, by direct aspiration atomic absorption spectroscopy, test, D 4834 (06.01) titanium dioxide content of pigments (recovered from whole paint), by atomic absorption spectroscopy, test, D4563 (06.01) Spectroscopy--atomic absorption antimony content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3717 (06.01) chromium content (low concentrations) in solids of liquid coatings/dried films, by atomic absorption spectroscopy, test, D 3718 (06.01) lead/cadmium/cobalt content (low concentrations) in nonvolatile portion of liquid coatings/dried films. by atomic absorption spectroscopy, test, D 3335 (06.01) mercury content (low concentrations) in liquid coatiflgs/coatings vehicles/dried films, by atomic absorption spectrascoDV test, D 3624 (06.01) Spectroscopy--x-ray fluorescence (XRF) sulfur content (of cellulosic materials), test D 2929 (06.02) titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D 4764(06,01) Specular gloss See Gloss Spirits of turpentine See Turpentine Spoilage See Stability--package > Spray-applied coatings So Coatings {headings) evaluating and comparing transfer conditions-laboratory conditions, test, D 5009 (06.01) transfer efficiency under production conditions for spray application of automotive paints, by weight basis, practice l) 5066 (06.01) ' -' Spray method testing industrial water-reducibfe coatings, guide, D 4712 (06.01) Spreading rate hiding power of paints, by reflectometry, test, A D 2805 (06.01) Stability--paints/related coatings/materials accelerated testing of paints/varnishes/lacquers/related products, using.filtered open flanje carbon-arc light/water exposure apparatus, practice, D822 (06.01) conducting tests on paint/varnish/lacquer/related products, using enclosed carbori-arc light/water exposure apparatus, practice, D5031 (06.01) copper phthalocyanine blue pigment, spec,, D 963 (06.02) estimating package stability of coatings for ultraviolet curing, test, D 4144 (06.01) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) ' heat stability ofcelliilose acetate, test, D 871 (06.02)' heat stability ofcellulose,ester, test, A D 817 (06.02) light stability ofclear coatings, by sunlight-through-glass method, test, D 2620 (06.01) package stability ofsolvent-reducible/water-reducible paint, test, D1849 (06.01) Staining effect of staining agents (on organic finishes in the automobile" industry), practice, D 1540 .(06.01) ; practical washdbility of organic coatings, test, D 4828 (06.01) stain removal (from multicolor lacquers on primed steei panels), test, D 2198 (06.01) stain resistance of fbctpjfy-applied coatings oh wobd products, practice, D 3023 (06.01) Standard color solutions See Color (headings) Static coefficient of friction See Coefficient of friction Statistical methods conducting interlaboratory study to determine precision of test method, practice, E 691 (06.03) Steam-distilled wood turpentine See Turpenfine Steel bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (86.01) Steel--panels paint and related coatings exposure tests, methods for preparation, D 609 (06.01) 1188 DUP0502 98364 Index of ASTM Standards, Section 6 preparation of hot-dipped nonpassivated galvanized steel panels for testing paint/varnish/laequer/related products, test, D2201 (06.01) Steel---substrates film thickness of pipeline coatings on steel, nondestructive measurement, method, G12 (06.01) Steel--surfaces assessing the condition of aged coatings on steel surfaces, guide, D 5065 (06.01) coating contractor qualification (for nuclear-powered generation facilities), practice, D 4286.(06.01) degree ofrusting on painted steel surfaces, method, AD 610 (06.01) evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A D 2485 (06.01) profile of abrasive blast-cleaned sieel surfaces, in laboratory/ field/fabricating shop, test, D 4417 (06.01) qualification ofjourneyman painters for application of coatings to steel surfaces of safety-related areas'in nuclear facilities, practice, D 4228 (06.01) Steel blue pigment See Iron blue Steel cubes bond strength of thermoplastic traffic marking, materials, using cement bricks/steel cubes, test, D 4796 (06.01) Steel panels paint and related coatings exposure tests, methods for preparation, D.609 (06.01) preparation of hot-dipped nonpassivated galvanized steel panels for testing paint/vamish/lacquer/related products, test, D 2201 (06.01) Steel samples sample preparation for qualification testing of coatings (Used in nuclear power facilities), spec., D 5139 (06.01) Step gages wet film thickness of organic coatings, by notched gages, practice, D 4414 (06.01) Sticking blocking resistance of trade sales paints, test, D 4946 (06.01) Stiffness free films of paints and related coatings, test, D 2370 (06.01) Stone--marble/limestone/sandstone/granite preparatory surface cleaning of architectural sandstone, practice, D 5107 (06.01) Stormer method consistency of paints, using Stormer viscometer, test, D 562 (06.01) sampling and testing pine tars/pine-tar oils, method, D 856 (06.03) Strength---general , .? colored pigments, by miniature sandmill method, te$t, A D 3022 (06.02) Strength--tinting colored pigments (dry/pastes in oil), using a mechanical muller, test, D 387 (06.02) relative tinting strength of white pigments, by reflectance measurements, test, D 2745 (06.02) relative tinting strength of white pigments, by visual observation, test, D 332 (06.02) Stress pull-off strength of coatings, using portable adhesion testers, test, D4541 (06.01) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, D 4939 (06.01) Strip test detection of copper corrosion from petroleum products, by copper strip tarnish test, A D130 (06.03) Stroke cure time stroke cure time of thermosetting phenol-formaldehyde resins, test, D 4640 (06.02) Sulfate content--pnints/relarod coatings Strontium chromate pigment : Sa Pigments (general properties) chemical analysis of strontium chromate pigment, test, D1845 (06.02) strontium chromate pigment, spec., D1649 (06.02) Structural applications--paint field identification of coatings, test, D 5043 (06.01) Styrene analysis of styrene by capillary gas chromatography, test, 05135(06.03) apparent density of industrial aromatic hydrocarbons, test, D 2935 (06.03) benzene content of cyclic hydrocarbon products, by gas chromatography, test, D 4534 (06.03) commercial density (of pure liquid chemicals), test, 0 3505.(06.03) perpjddsSjiniStyrepe monomer, test, D 2119 (06.03) peroxides in stvrene monomer, test, D 2119 (06.03) polymer content of styrene monomer, test, D 2121 (06.03) /Hert-butylcatechol (TBC) in styrene monomer, test, D 2120 (06.03) purities/impunties, by gas chromatography, test, D 3962 (06.03) purity of hydrocarbons from freezing points, test, D1016 (06.03) * purity of styrene, by freezing point method, test, D 3799 (06.03) residual p-tert-butylcatechol (TBC) in styrene monomer, by addition of NaOH, test, D 4590 (06.03) sampling/handling liquid cyclic products (at ambient temperature), practice, D 3437 (06.03) styrene monomer 996, spec., D 2827 (06.03) unreacted monomer content of latexes, by gas-liquid chromatography, test, D 4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) Styrene-butadiene coatings systems dichloromethane/l,l,l-trichloroethane content in paints/ coatings, by.direct injection gas chromatography, test, D 4457 (106.01) water content of water-reducible paints, by direct injection into gas chromatograph, test, 113792 (06.01) Subsieve analysis See Sieve analysis:--subsieve (headings) Substrates--coating applications accelerated outdoor exposure tests of coatings (applied to metal substrates), practice, D4141 (06.01) adhesion of coating films to metallic substrates, by tape test, D 3359 (06.01) ' adhesion of organic coatings to-plastic substrates, by direct tensile testing, D 5179 (06.01) discontinuity (holiday) testing of nonconductive protective coating on metallic substrates, practice, D5162 (06.01) mandrel bend test of attached organic coatings, test, D 522 (06.01) painting inspectors (metal substrates), guide, Q3276 (06.01) paint spatter resistance to roller application, test, D 4707 (06.01) preparation of free films of organic coatings, practice, D 4708 (06.01) specifying inspection requirements for coating/lining work on , metal substrates, guide, D 5161 (06.01) testing solvent-borne architectural (interior/exterior) coatings, guide, D5146 (06.01) Sulfate ash content pentaerythritol (for manufacture of alkyd/other synthetic resins), tests, D 2195 (06.03) Sulfate content--paints/related coatings acid-insoluble extenders in (iron/copper phthalocyanine/ ultramarine) blue pigments, test, D 1135 (06.02) cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, D 871 (06.02) 1189 DUP050298365 Index of ASTM Standards, Section 6 Slilfate contentfPpainte/related coatings lead peroxirfc/true red lead content ofdry red lead pigments, test, D 49 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, test, D 126 (06.02) * Sulfated ash content ashing cellulose, test, D 3516 (06.02) ethylcellulose, test, D 914 (06.02) Sulfate white lead pigments See Basic sulfate white lead Sulfate wood turpentine See Turpentine Sulfide content sulfide in white pigment separated from solvent-reducible paints, test, 0 2351 (06.02) Sulfur content cellulose acetate propionates/butyrate, test, A D 817 (06.02) cellulose acetate, test, 0 871 (06.02) cellulosic materials, by X-ray fluorescence, test, D 2929 (06.02) sulfur (trace quantities) in liquid aromatic hydrocarbons, by oxidative microcoulometry, test, 0 3961 (06.03) zinc dust (metallic zinc powder), test, 0 521 (06.02) Sulfur content--petroleum products mineral (petroleum) spirits hydrocarbon .drycleaning solvent, spec., 0235 (06.03) " sampling/handling 4,4- isopropylidene diphenol (bisphenol-A), practice, D 4297 (06.03) Sulfur dioxide (S02) content qualitative, of industrial aromatic hydrocarbons, test, D 853 (06.03) sulfur dioxide in white pigment separated from solvent- reducible paints, test, Q 2352 (06.02) Sunflower oil sunflower oil (once-refined, technical grade), spec., D 3169 (06.03) f Sunlight/monochromatic light exposure lightfastness ofpigments (in artists' paints), test, D 4303 (06,01) Surface analysis--paints/related coatings/materials gloss differences between surfaces of similar appearance, method for visual evaluation, 0 4449 (06,01) gloss of high-gloss metailic/riomhetallic surfaces, by goniophoto- metiy, method, E 430 (06.01) printing inks/ink films/related materials, selecting test methods, guide, 0 5010 (06.01) profile of abrasive blast-cleaned steel surfaces, iii laboratory/ field/fabricating shop, test, 0 4417 (06.01) pull-off strength ofcoatings, using portable adhesion testers, test, 04541 (06.01) static friction of Coating surfaces, test, 04518 (06.01) subjecting marine antifouiing coating to bifouling and fluid shear forces in natural seawater, test, 04939 (06.01) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, 0 3259(06.01) Surface preparation--paints/related coatings Sa Specimen preparation (for testing)--paints/related coatings preparation of hot-dipped nonpassivated galvanized steel panels for testing paint/varnish/lacquer/related products, test, 0 2201(06.01) preparatory surface cleaning of architectural sandstone, practice, 0 5107(06.01) standard pictorial surface preparation standards for painting steel surfaces, A 0 2200 (06.01) Surfacers See Primer I' Surfaces (of nuclear facilities) coating contractor qualification (for nuclear-powered generation facilities), practice, 0 4286 (06.01) qualification ofjourneyman painters for application of coatings to concrete surfaces of safety-related areas in nuclear facilities, practice, D4227 (06.01) qualification ofjourneyman painters for application of coatings to steel surfaces of safety-related areas in nuclear facilities' practice, 0 4228 (06.01) Surface water resistance < ' See Resistance--water Surveillance establishing procedures to monitor performance of safety related coatings in operating nuclear power plant, guide, 05163(06.01) " Suspension fluids flash point (offuel oils/lube oils/suspension ofsohds/Uquids), by Pensky-Marteus, dosed tester, test, 0 93 (06.03) Sustained burning test sustained burning (of liquid mixtures), by Seta-flash tester (open cup), test, 0 4206 (06,01,06.03) sustained burning (of low viscosity liquid mixtures), by Wick test, D 4207 (06.03) Swelling dear/pigmented organic coatings, test, 0 1308 (06.01) Swelling and Cracking edge performance ofcomposite wood products under surfactant accelerated moisture stress, test, 0 2065 (06.01) Synthetic amyl alcohol' / amyl alcohol (synthetic), spec., 0 319 (06.03) Synthetic black iron oxide (magnetite) See Iron oxide black Synthetic drying oils See Oils--drying Synthetic ethylhexanol See 2-Ethylhexanol Synthetic hematite (red) See Iron oxide red Synthetic phenolic resins See RCsihs--phenolic Synthetic pine oil See ' Oils--pine (natural/synthetic) Synthetic primary amyl acetate See Primary amyl acetate Synthetic yellow iron oxide See Iron oxide yellow T- Tack apparent tack of printing inks/vehicles, by inkometer, test, 04361 (06.01) Tag closed-cup tester flash point by Tag dosed tester, test, 0 56 (06.03) Tag open-cup tester flash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) Talc (pigment) See Magnesium silicate Tali oil/tall oil rosin tall oil, methods of testing, D 803 (06.03) volatile resin acids in tail oil/gum/wood rosin, by gas chromatography, test, D 3008 (06.03) Tank cars/wagons/other shipping containers See Containers--tank cars/wagons Tanks cresyiic acid and phenol, practice, D 3852 (06.03) sampling and handling aniline, practice, D 3436 (06.03) sampling/handling liquid cyclic products (af ambient temperature), practice, D 3437 (06.03) 1190 ri?1 ' I DUP050298366 Index of ASTM Standards, Section 6 Thickness--paints/related coatings/materials Tar adds color of cresylic acids ("C" series standards), test, D 3627 (06.03) gel time, test, D 2870 (06,03) phenol content (pf tar acid mixtures), by gas liquid chromatog raphy* test, D 3626 (06.03) TBC inhibitor p-rert-butylcatechol (TBC) in styrene monomer, test, D 2120 (06.03) residual p-tert-butylcatechol (TBC) in Styrene monomer, by addition of NaOH; test, D 4590 (06.03) " TDI content See Free toluene diisocyanate content Temperature (application) bond strength of thermoplastic traffic marking materials, using cement bricks/steel cubes, test, D 4796 (063)1) chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) Temperature service applications--high conducting tests on paint/vamish/lacquer/related products/ using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) Temperature tests--paints/related coatings/materials evaluating (interior/exterior) coatings for protecting steel surfaces at high-temperature service, test, A D 2485 (06.01) exposure of paints/related coatings to fluorescent UV- condensation light-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) freeze-thaw resistance ofwater-borne coatings, test, D 2243 (06.01) low-temperature coalescence (oflatex paint films), test, D 3793 (06.01) minimum film formation temperature (MFFT) of emulsion vehicles, test, D 2354 (06.02) nonvolatile content of latexes, test, D 4758 (06,02) operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D 4451 (06.01) solidification point of 4,4* isopropylidenediphenol (Bisphenol A), test, D 4493 (06.03) temperature-change (high-low) resistance of clear nitrocellulose lacquer films applied to wood, test, D1211 (06(01) temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (06.01) Temperature tests--plastics operating light-exposure apparatus (xenon-arc type) with/ without water for exposure of nonmetallic materials, practice, G 26 (06.01) Ten-degree xylene (10 xylol) See Xylene (ten-degree) Tension (tensile) properties/tests--paints/related coatings adhesion of organic coatings to plastic substrates, by direct tensile testing, D 5179 (06.01) paints/related coatings (free films), test, D 2370 (06.01) preparation of free films of organic coatings, practice, D 4708 (06.01) Terminology--paints/related coatings/materiais aromatic hydrocarboqs/related chemicals, terminology, D 4790 (06.03) cellulose/cellulose derivatives, terminology, D1695 (06.02) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) paint/vamish/lacqtier/related products, terminology, D16 (06.01,06.02, 06.03) Terpene alcohols content sampling and testing pine oil, method, D 802 (06.03) Terpene solvents Sa Solvents (headings) sampling and testing dipentene, method, D 801 (06.03) Terra alba See Calcium sulfate content Terra di sienna See Sienna(burnt add raw) Testing methods recording results on single-/multi-panel forms, method, A D1150 (06.01) Testing methods--paints/related coatings See Guides for testing paints/related coatings/materials Test samples sample preparation for qualification testing of coatings (used in nuclear power facilities), spec.;- D-5139 (06.01) Test specimens See Specimen preparation (for testing) (headings) Tetraethylammonium bromide titanium dioxide content in paint; by x-ray fluorescence spectroscopy, test, D 4764 (06.01) Texture gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) Thawing See Freezing and thawing Thermal black See Pigments--carbon black Thermal degradation and endurance cellulose acetate, test, D 871 (06.02) soluble cellulose nitrate, testing,, methods, D 301 (06.02) Thermal transmittance See Transmittance and reflectance Thermal voltaic-type infrared radiation thermometers temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, D 3259 (06.01) Thermistor-type,infrared radiation thermometers temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, 1)3259(06.01) Thermometers thermometer specifications for flash point (of fuel oils/Iube oils/suspension of solids/liquids), by Pensky-Martens closed tester, test, D 93 (06.03) Thermoplastic traffic marking evaluation of color for thermoplastic traffic marking materials, test, D 4960 (06.01) Thermoplastic traffic marking material . chemical/gravimetric analysis of white/yellow thermoplastic traffic marking material containing lead chromate and titanium dioxide, test, D 4797 (06.01) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D 4451 (06.01) Thermosetting materials/properties--resins stroke cure time of thermosetting phenol-formaldehyde resins, test, D 4640 (06.02) Thermosetting phenol-formaldehyde See Phenolic resins . Thickness--paints/related coatings/materials dry film thickness, of nonmagnetic coatings (paints/ vamish/lacquer) applied to a ferrous base, D 1186 (06.01) dry film thickness of protective coating systems, by destructive means, test, D 4138 (06.01) erosion testing of antifouting paints, using high velocity water, test, D4938 (06.01) producing films of uniform thickness of paint/vamish/related products on test panels, test, D 823 (06.01) subjecting marine antifouling coating to bifouiing and fluid shear forces in natural seawater, test, D4939 (06.01) 1191 s iii Stlsis DUP050298367 Index of ASTM Standards, Section 6 Thickness--paints/related coatings/materials wet film thickness of organic coatings, by notched gages, practice, D4414 (06,01) , Thintiers (paint) See Paint--thinners Thiophene content refined benzene, by gas chromatography (with flame photometric detection), test, 0 4735 (06.03) thiophene content of benzene, by spectrophotometry; test, 1685 (06.03) Thiosulfate method chromium content of strontium chromate pigment, by tliiosulfatp,method, test, D1845 (06.02) Thixotropy rheological properties ;of non-Newtonian materials, by rotational (Brookfield) viscometer, test, 02196 (06.01) .;, Three-degree xylol (3 xylol) See Xylene (nitration .grade) ' Time tests ... amount of liquid separated as upper,layer from. 3 viscous.. * solution/dispersion containing dispersed solids, test,. - 0 4948(06.01) Tinting strength colored pigments (dry/pastes in oil), with a mechanical muiler, test, D387 (06.02) relative tinting strength ofchromatic paints, test, D 4838'(06.0I) relative tinting strength ofprinting ink dispersions, tesf, 02066(06.01) relative tinting strength of white pigments, by: reflectance ! measurements, test, 0 2745 (06.02) ' relative tinting strength of yvhite pigments, by visual , ' obsefvafion, test,10 332 (06;02) 1 Titanium content white titanium pigments, chemical analysis, test, 01394 (06.02) Titanium dioxide slurries weight percent of solids in aqueotis 'slurries oftitanium, dioxide pigments, test, 0 3926 (06.02) " Titanium dioxide (TiO,) ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, tiest, 0 3720(06.02)';i ` relative tinting strength of white pigments, by reflectance, measurements, test, 0 2745 (06.02) titanium dioxide content in paint, by x-ray fluorescence spectroscopy, test, D 4764-(06.01) titanium dioxide content of pigments' (recovered from whole paint), by atomic absorption spectroscopy, test, ' 04563(06.01) titanium dioxide pigments, spec., 0476 (06.02) . weight percent of solids in aqueous slurries of titanium dioxide pigments, test, D 3926 (06.02) white titanium pigments, chemical analysis, test, 01394 (06.02) Titer " 1 solidification (titer) poiat of fattjf acids, test, 01982 (06.03) Titrimetric method ,f resin solution dilutability, test, D 5062 (06.03) Toluene ,, acidity of benZene/tdluene/Xylcttes/soliient naplithas/similar industrial aromatic hydrocarbons, test, 0 847 (06.03) acid wash color, test, 0 848 (06.03) apparent density of industrial aromatic hydrocarbons; test, 0 2935(06.03), aromatic hydrocarbons/related chemicals, terminology,' 04790(06.03) benzene content of cyclic hydrocarbon products; by gas chromatography, test, 0 4534 (06.03) ?' commercial density (of pure liquid chemicals); test, 0 3505(06.03) distillation, test, 0850 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, 0 5060 (06.03) nitration grade toluene, spec., D 841 (06.03) purity of hydrocarbons from freezing points, test, 01016(0603) sampling/handling liquid cyclic products (at ambient temperature), practice, D3437 (06,03) soluble cellulose nitrate, testing, methods, 0 301 (06.02) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, bygp chromatography, test, 0 2360 (06.03) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, 05194 (06.03) . volume/weighi of industrial aromatic hydrocarbons, method, 01555(06.03) xylene isomer analysis, by gas chromatography, test, 02306(06.03) Toluene insolubles content toluene-insoluble soUd matter (santychips/dirt/bark) in rosin, test, 0 269 (06.0:3) Totuidine red m . -u pure toluidine red toner, spec., D 656 (06.02) . Toluidine red pigment para.red/toiuidine red pigments; testing, D 970 (06.02) Toner (para/toluidine red) para red/toluidine red pigments, testing, D 970 (06.02) Top liquid layers' - amount pf liquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, 04948(06.01) ' Total efttoride content : See Chloride content(headings) Total nitrogen oxides content See Nitrogen oxides ... Total sulfur content See Sulfate content (headings) . Total titanium :. ' total titanium inrivhitetitaniUm pigments, by Jones reduetor/aluminum reduction'method, test, 01394 (06.02) Toxicity/toxicology ' unreacted monomer content of latexes; fry gas-liquid chromatography, test, 04747 (06.02)' ` Trace clemepts contents , ' sulfiif^trabfe quantities) in liquid'aromatic hydrocarbons, by . oxidative micropoulpmetry.jtest, p 3961 (06)03) Trace elements contents--chloride , 5<z C)ilpride content {headings) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, 0 5194 (06.03) Trace impurities content ----- See Impurities content . . Sai Purity Trace lead/cadmium/cobalt paint lead/cadmium/cobalt content (low concentrations)!!) nonvolatile portion of liquid coatings/dried films, by atomic absorption spectroscopy, test, 0 3335 (06.01) Trace monomers unreacted monomer content of latexes,* by gas-liquid chromatography, test, 04747 (06,02) Trade sales paint blocking resistance of trade sales paints, test, 0 4946 (06.01) Traffic marking materials evaluation of color for thermoplastic traffic marking materials, test, D 4960 (06.01) Traffic paint evaluating degree of bleeding of traffic/pavement marking paint, test, A 0868 (06.01) evaluating degreeofchipping, A 0913 (06.01) ' glass spheres in, test for roundness, D1155 (06.02) laboratory evaluation ofdegree of bleeding of traffic/pavement ; marking paint; test, 0 969 (06.01) 1192 DUP0502 98368 Index of ASTM Standards, Section 6 Uretlfines laboratory test for settling properties, during storage, D1309 (06.01) methods of conducting road service tests on, D 713 (06;01) no-pick-up time (drying time), test, D 711 (06.01) pigment content of paint/traffic marking material, by low-temperature furnace ashing, test, D 4451,(06.01) practices for testing, D 2205 (06.01) sieve analysis of glass spheres (for relroreflective pavements markings/industrial uses), test, D1214 (06.02) solvent and fuel resistance, test, 0 2792 (06,01) uniformity of vehicle soiids (by spectroscopv/gas chromatog raphy), selection and use of test procedures, practice, D 2743 (06.01) Transesterification identification of carboxylic acids in alkyd resins D 2455 (06.02) Transfer efficiency (TE) evaluating and comparing transfer conditions-laboratory conditions, test, I> 5009 (06.01) transfer efficiency under production conditions for spray., . application of automotive paints, by weight basis, practice, D5066 (06.01) Transparent liquids See Liquids Tributyl tin (TBT) < organotin release rates of antifouling coating systems in sea water, using graphite furnace atomic absorption spectrophotometry (GF-AAS), test, D 5108 (06.01) Trichloratrifluoroethane-extractable matter permanganate time of acetone/methanol, test, 01721 (06.03) unsaponifiable matter content, test, D1399 (06.03) Tricresyl phosphate tricresyl phosphate, spec., D 363 (06.03) volatile matter in tricresyl phosphate, test, D1468 (06,03) Tristimuius valne Sa Color (headings) calculation of color differences from instrumentally measured color coordinates, test, D 2244 (06.01) directional refieetdride factor (45-deg 0-deg) of opaque specimens, by broad-band filter reflectometry, test, , E 97 (06.01) True red lead lead peroxide/true red lead content of dry red lead pigments, test, D49 (06.02) Tung oil See Oils--tung .... Tunnel method small-scale evaluation of fire-retardant painis, by 2-foot tunnel method, test, D 3806 (06.01) Turbidimetric method reporting particle size characteristics of pigments, practice, D1366 (06.02) Turbidity resin solution dilutability, test, D 5062 (06.03) Turkey red See Iron oxide red ' Turkish umber See Umber (burnt and raw) Turpentine pinene composition, by gas chromatography, test, D 3009 (06.03) sampling and testing turpentine, method, D 233 (06.03) spirits of turpentine; spec., D 13 (06.03) Twenty-four hour testing amount of liquid separated as upper layer from a viscous ' solution/dispersion containing dispersed solids, test, D 4948 (06.01) Two-foot tunnel method small-scale evaluation of fire-retardant paints, by 2-foot tunnel method, test, D 3806 (06.01) u Ultrafiltrates add/base milliequivalent content of (anodic/cathodic) electrocoat baths/their ultrafiltrates, test, D 4370 (06.01) apparent pH of electrocoat baths, test, 0 4584 (06.01) electrical conductivity of electrocoat baths, test, D 4399 (06.01) nonvolatile a&ti,pigment content qf electrocoat baths, using muffle furnace, test, D 5145 (06.01) Ultramarine blue pigment chemical analysis of(iron/copper phthalocyanine/ultramarine) blue pigments, test, 0 1135 (06.02) chemical analysis of phthalocyanine blue/green pigments, test, D 3256 (06.02) ultramarine blue pigment, spec., 0 262 (06.02) Ultraviolet-cured coatings cure time, practice for reporting, D 3732 (06.01) estimating package stability of coatings for ultraviolet curing, test, 04144 (06.01) Ultraviolet (UV) light/radiation accelerated testing ofpaints/vamishes/lacquers/related products, using filtered open flame carbon-arc light/water exposure apparatus, practice, 0 822 (06.01) conducting tests on paint/varnish/lacquer/related products, using enclosed carbon-arc Kght/water exposure apparatus, practice, D 5031 (06.01) exposure of paints/related coatings to fluorescent UVconrtensdtidii fight-water-exposure apparatus, practice for conducting tests, D 4587 (06.01) Umber (burnt and raw) chemical analysis of yellow/orange/red/brown pigments containing iron/maganese, test, 1> 50 (06.02) raw/burnt umber pigments, spec., 0 763 (06.02) Underground environments cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) Uniform thickness (of paints/related coatings) See Thickness--paints/related coatings/materiais Unloading tank cars/wagons/other shipping containers cresylic acid and pUenol,1 practice, 03852 (06.03) naphthalene,oiSalfeic/plithalic anhydride, practice, D3438 (06.03) sampling and handling aniline, practice, 0 3436 (06.03) Unreacted monomer content unreacted monomer content oflatexes, by gas-liquid chromatography, test, D4747 (06.02) unreacted monomer content of latexes using capillary column gas chromatography, test, D 4827 (06.02) " Unsaponifiable matter content alkyd resins and resin solutions, test, 01397 (06.02) rosin, test, D1065 (06.03) tali oil; methods of testing, D 803 (06.03) tricresyl phosphate, test, 01399 (06.03) unsaponifiable matter in drying oiis/fatty acids/polymerized fatty acids, test, D 1965 (06.03) Unsaturation drying oils/derivatives total, by modified RosenmundKuhnhenn .method, test, D1541 (06.03) drying oils/derivatives Wijs method, test, 01959 (06.03) Up and down method impact resistance of pipeline coatings, by falling weight test, G14 (06.01) Upper liquid layer amount ofliquid separated as upper layer from a viscous solution/dispersion containing dispersed solids, test, D 4948 (06.01) Urethanes isocyanate group content of urethane materials/prepolymers, test, D 2572 (06.02) 1193 T l is I DU P0502 98369 Urethanes Index ofASTMStandafds, Section 6 unreacted toluene diisocyanates in urethane prepolymers/ coating solutions, by gas chromatography, test, D 3432 (06.02) Urethanes--coatings ,. 2-eflibxyethyl acetate (99 % grade?), spec., D'372`8 (06.03) isocyanate group content of urethane maierials/prepblymersj test, t) 2572 (06.02) : ;77'.'' unreacted toluene diisocyanates iii urethan'e prepolymers/ coating solutions, by gas chromatography, "test, " D 3432 (06.02) , , i^ Vanadium content ' ~* paint driers, by EDTA method, test, D 3988 (06.03) '> Vapors ^ :H chemical resistance of pipeline costings, test, G 20 (06.01) : preparation of-free1 films'of organic coatings, practice,: D 4708 (06.01) 5 *'" Variances in manufacturing process samplirigindustrial'cheimcais.anriex, practice, E300 (06.03)' Varnish "' c '" acidity in volatile solvents/chemical intennediates (used in pairil/varhish/lacquer/related products), test, D1613 (06.03) conducting tests on paint/varnish/lacquer/related products, using eticlosed carbon-arc'li^ht/vyater bxptssure apparaius, practice, D 5031 (06.01) . ,s Varnishes ,7 77,,,,, abrasion resistance, by air blast abrasion test, A D 658 (06.|)1) abrasion resistance, of organjd coatings, by falllhjgabrasive,' D 968 (06.01) / . .. v, accelerated testing 6f paints/vamishes/lacqUers/reiated products, , using filtered open flame carbon-arq light/VratereX^Bsiife?"'' apparatus, practice:, 0822 (06.01) ! .: ; 7 7 ' ' acid value of organic coating materials, test, D 1639 (06.01) adhesion (to smooth paiiel surfaces), by scrape adhesibn test,* D 2197 (06.01) :' - clarity/cleannessof (npnpigmenteid) painfcand ink liqttidsjiby '- visual examination, test, D 2090 (06.02,,06.03) ,t` ,, clear/pigmented organic coatings, test,; 01308 (06.01) , color of transparent liquids, by Gardner color scale; test, D1544 (06.01, 06.02, 06.03) v discoloration (light stability), test, D 2620(06,01) , , dried varnish filmsi test, 0.1647,{06,01) dry film thickness of.noneonductive coatings (appliedctpi, , nonfereous metal base), nondestructive rneasuretoertViteSt, D 14no-(06.01) dry-film thickness of organic coatings, using, micrometers, test,, , D1005(06;01) ... r. 777) elasticity/toughness of varnishes, test, JD 1642 (06.01j t 777 elongation/tensile strength/stipiess; test, D 2370 (06,01): 7- exterior durability, test, D1641 (06.01) : 7 7,, film formation rates in drying or curing process, ht room temperature, test, D1640 (06.(11) flash point of liquids, by Setaflash closed-cup apparatus, test,. D 3278 (06.03) , , ,'7 gas checking and draft test, 0 1643 (Q6.0I) ... glacial acrylic acid(99.6 % grade), spec., D 4416 016,0$) ' . high shear viscosity (of paints/vaniishes/related product^), by ICI cone/plate viscometer, rest, D 4287 (06.01)' ' . 7 indentation hardness of* organic coatings, by Kr.oop' and Pfund methods, test, D1474 (06.01) liquid paint driers, selection of test methods, D 564 (06:03) methyl* n-hmyl ketone (98 % grade), spec., 0 4360 (06.03)- moisture vapor transmission of organic coating' films; te'sf, 01653(06.01) : v* nonvolatile matter content, test, D1644 (06.01) paint-and related coatings exposure tests; methods for preparation, D609 (06.01) paint/vamish/iacquer/related products, terminology, D 16 (06.01, 06.02, 06.03) paint/Varnish/iacquer/related products, test, A 01475 (06.01) preparation offree films of organic coatings,' practice, 04708(06.01) preparing glass panels for tasting, 03891 (06.01) qualitative detection of rosiw fe varMifies, by LSsberman- Storch/Halphen-Hicks tests, D1542 (06.01, 06.02) rosin acids contenf, test, 0(l46b (06102) sampling and testing shellac Varnish,D1650 (06.02) selefc'don and use Oftest proebdures, b 154 (06.01) specific gravity at?i25/25<j, test, D 1963!'(06.tl3) standard environments for ponditioning/testlug'paint/ , varpish/lacquer/related materials, spec.., 0 3924 (06101)* ' steelSuffaces, resistance to failurc,',by: water immersion test, D 870 (06.01) testing watei' resistance ofcoatings at 1001 > relative humidity, practice, D2247 (06.01)' ; ` - viscosity of paints/varnisheS/lactjuers, by Ford'viscority clip, test, D1200 (06.01) viscosity (of paints/varnishes/lacquers/related material!), by dip-type viscosity cups, test, D 4212 (06.01) ' volatile content in phenolic resins, test, D 4639 (06.02) volatile/nonvolatile content (of cellulosics/emulsions/resin solutions/shellac/varnishes), selecting test procedure, practice, D 4209 (06.02) wet film thifckness 6forganic Coatings, D1212 (06.01) wet film thickness of organic coatings,.by notched gages; -w, tedpf&ctice,?0)4414 (06.01) , -r artists' paints (oil/resin-oil/alkyd), spec., D 4302 (06.01) .; *-i`f Vehicles ., nonvolatile:'coHent of printing irilcs/re'siri solutions/vehicles, test, D 4713 (06.01) ' vU Vehicle separation--solvent-type paints ; 7 ?, amount of liquid separated asi,upper,layer from a viscous ` solution/disperiioh containing .dispersed solids) test, D4948 (Q6.oi) / ;7'7 7!`7/;'`7 "v high-speed centrifuge, for pi&nent'conterit, test 0 2698 (06.01) infrared identification of vehicle solids from solvent-reducible paints, by,infrared,spectroscopy, test, D 2621 (06.0l) *' ` pigment conVent of solvent-reducible paiftts, fest, 02371 06:01) vacuum distillation (for vehicle separation In sblvent-tjlpe paints), practice, D 3272 (06.01) vs > vehicle separation'from solvent-reducible pahits, by centrifuge, , practice, 0 2372 (06.01) Vehicle solids content' '' 7-, See Solids content . 7, . " 'i` Venetian red ...r, . . . 7 7 7 ""7 J chemical analysis ofye'irbw/drange'/reS/brownj pigments `'' containing iron/maganese, test, D 50 (06.02) .. Vinylacetate ,r ,, 77 acetaldehyde content of vinyl acetate,' test, 0 2191 (6`6.oj3)7 1 acidity in vinyl acetate and acetaldehyde, test, P 2086 (06.03) ' hydroquinone in vinyl acetate, test, 0 2193t06)o8) vinyl acetate, spec., 0 2190 (06,03) . ,' Vinyl antifouling coatings See Antifouling coating systcm. ; Vinyl chloride monomer (residual) content >. - residual vinyl chloride monomer content of.poly(vinyl chloride) resins/compounds/copolymers by, solution injection technique, test, D 3680 (06.02) . Viscometers--Brookfield rheological properties of, non-Newtonian materials,,by,rotational (Brookfield) viscometer, test, 0 2196 (06.01) Viscometers--falling rod viscosity of printing inks/vehicles, by falling-rod viscometer, test, D 4040 (06.01) 1194 DUP050298370 Index of ASTM Standards, Section 6 Volatile matter content Viscometers--Ford viscosity of paints/vamishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) Viscometers--Gardner-Holdt tail oil, methods- of testing, D 803 (06.03) Viscometers--ICI cone/plate high shear viscosity (of paints/varnishes/related products), by ICI cone/plate viscometer, test, D4287 (06:0t) Viscometers--Saybolt " viscosity of pine tars/pine-tar oils, by Stormer/Saybolt Furol - viscometeis, test, D856 (06.03) ! Viscometers--Stormer viscosity of pine tars/pine-tar oils, by Stormer/Saybolt Puiol viscometers, test, D 856 (06.03) Viscometers--Weissenberg Rheogonioineter viscosity of polynieric powdetsypowifer cSatiiigs, test, D 3451 (06.01) :/ ' ........ '-f "' ! Viscometers--Zahn coil coatings, testing, practice, D 3794 (06.iBfl) Viscosity--paints/related coatings/materials ' cellulose acetate propionates/butyrate, test,!\.D 817 (06.02) cellulose acfet$ite, test, D 871^(06.02) coil coatitigs; testing, practice', D3794 (06.01), comparison of the brush drag of latex paints' test,, , D 4958 (06.01) J consistency of paints, using Stormer viscometer, test, D 562 (06.01), . ; dip-type viscosity, (nip, test,'&4212 (06.01) f ethylcqllulose, test, D914 (06,102) , high shear viscosity (of paints/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) hydrogen sulfide/sulfur dioxide (Oualttit^tlve) of industrial' aromatic hydrocarbons/ test, 0 23:63 (06.02) hydroXyethylcellulose, test, 1!>'2364,(0&02) intrinsic viscosity of cellulose, test, D 1795 (06,02) methyleellulose, test, D 1347 (06.02) ' .> paints/varnishes/lacquers, by Ford viscosity cup, test, D1200 (06.01) ' polymeric powders/powder coatings, by Weissenberg ` " rheogoniometer; test, D 3451 (06.01) resin solutions, test, D 1725 (06.02) -vr- rheological properties of non-Newtonian materials, by rotational (Brookfield) viscometer, test, D 2196 (06.01) , ,. rosin oil, test,,D 1131,(06.03) sodium glycolate content of sodium carboxymethylcellulosc, test,,,D 1435U0P.02) ,; soluble cellulose nitfate,-,testing, methods, D 301 (06.02), soluble nitrocellulose base solutions, test, D 365 (06.02) tall oil, methods of testing, D 803 (06.03) transparent liquids, by bubble-dome method, test, D1545 (06.01, 06.02, 06.03) viscosity ofcellulose derivatives, by ball-drop method, test, D1343 (06.02) viscosity ofpaints/related materials, by ISO flow cups, test, D 5125 (06.03) viscosity*of pine fars/pine-tar oils, by Stormer/Saybolt Furbf viscometers, test, D 856 (06.03) viscosity'of printing inks/vehicles, by falling-rod VisCotneter, ~ test, D 4040 (06.01) Wick test (for low viscosity liquids) D 4207 (06.03) Viscosity at high shear high shear viscosity (of paints/varnishes/related products), by ICI cone/plate viscometer, test, D 4287 (06.01) Viscous liquids/materials flash point (of fuel oils/lube oils/suspension o solids/liquids), by Pensky-Martens closed tester, test, Q 93 (06.03) liquid/solid status (of viscous materials), test, D 4359 (06,01) Visual examination--paints/felated eoatings/materials darity/cleanness of (nonpigmented) paint and ink liquids, by : visual examination,1 test, ;D 2090 (06.02, 06.03) color of cresylic acids (<lC" series standards), test, D 3627(06.03) color (of nttdeie anhydride/phthaiic anhydride--in molten state and after heating), by platinum-cobalt scale, test, B3itSiD03) - color (of solid aromatic hydrocarbons/related materials--in molten state), by platinum-cobalt scale, test, D1686 (06.03) evaluating;ddjjjree' of bleeding of traffic/pavement marking paint, test, A D 868 (06.01) evaluation of painted/coated specimens subjected to corrosive environments, method, D 1654(06.01) formability/adhesion of zinc-rich primer/chromate complex coatings (ob steel), test, D 4146 (06.01) freeze-thaw resistance of water-borne coatings, test, D 2243 (06.01) gloss differences between surfaces of similar appearance, method for visual evaluation, D 4449 (06.01) gloss/sheen uniformity evaluation; test, D3928 (06.01) laboratory evaluation of degree of bleeding of traflic/pavement marking paint, test, D 969: (06.01) MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) porosity of paint films (to indicate coating penetration), test, D 3258 (06.01) relative tinting strength of white.pigments, by visual observation, test, D 332 (06.02) solution color of 4,4'-isopropylidenediphenOl (dissolved in methanol), test, D 4789 (06.03) subjecting marine antifouling coating to bifouling and fluid shear forces in natural seawater, test, p 4939 (06.01) testing industrial .vpter-reducible coatings, guide, D 4712 (06.01) wet-to-diy hiOing chaiige of architectural coatings, test, 0 5007(06.01) Visual examination--pipeline coatings cathodic disbonding of pipeline coatings, accelerated procedure, test, G 8 (06.01) effects df &utdhor weathering on pipeline coatings, test, G11 (06.01) impact resistance of pipeline coatings, by limestone drop test, G 13 (06101) VM & P naphthas VM & P naphthas, spec., D 3735 (06.03) VOC abatement amount of volatile organic compound (VOC) released from solventborne automotive coatings and available for removal in a VOC control device (abatement), test, D 5087 (06.01) VOC calculation volatile organic content (VOCJ'of paints/related coatings, selecting test procedures, practice, D 3960 (06.01) Volatile acids content sampling and testing pine tars/pine-tar oils, method, 0 856(06.03) Volatile liquids : low viscosity,,rate of evaporation, test, D 3539 (06.01) Volatile matter content - calcium borosilicate, test, D 4487 (06.02) cellulosics/emulsions/resin sqlutions/sheliac/vamishes, selecting test procedures, practice, D 4209 (06.02) driers/drying oils/naval stores and solvents, selecting test procedures, guide, D 4140 (06.03) hygroscopic moisture (and other matter volatile under test conditions) in pigments, test, D 280 (06.02) loss on heating ofdrying oils, test, D 1960 (06.03) moisture content of pigments, D1208 (06.02) paint/raw paint material, practice, D 2832 (06.01) paints (solvent-reducible), test, D 2369 (06.01) sampling/testing lac resins (orange shellac/button lac/garnet lac/bleached lac), test, D 29 (06.02) 1195 DUP050298371 Volatile matter content Index of ASTM Standards, Section 6 sampling/testing volatile solvents/chemical intermediates (for paints/lacquer/vamish/related material)* selecting test methods, D 268 (06.03) volatile content in phenolic resins, test, D 4639 (06.02) volatile matter in tricresyl phosphate, test, D1468. (06.03) volatile/nonvoiatile content (of pigments), selecting test procedures, guide, D4139(06.82) volatile organic content (VOC) of paints/reiated qpdjngss selecting test procedures, practice, 03960 (06.01) Volatile organic compounds (VOC)--paints/reiated coatings dichloromethane/1,1,1 -trichloroethane content in paints/ coatings, by direct injection gas chromatography, test, 04457 (06.01) distillation range (between 30 and 350Q of volatile organic liquids, test, D1078 (06.03) nonvolatile content in silanes/siloxanes/siiane-siloxane blends used in masonry water-repellent treatments* test, 0 5095 (06.01) nonvolatile content of resin solutions (in volatilerorganic , solvents), test, 0 1259 (06.02) volatile oil in rosin, test,-D 889 (06.03) volatile organic compounds (VOC) of solvent reducible paints in aerosol cans, test, D 5200 (06.01) volatile organic content (VOC) of paints/reiated coatings, selecting test procedures, practice, D 3960,(06.01) Volatile organic compounds (VOC)--paints/reiated materials calculating formulation physicabconstants of.paints/coatings, practice, D 5201 (06.01) Volatile resin acids content See Resins (headings) Volatile solvents (in paints/coatings) See Solvents--paints/reiated coatings/materials Volatility distillation range (between 30 and 350C) of volatile organic liquids, test, 01078 (06.03) Volume--petroleum products volume/weight of industrial aromatic hydrocarbons, method, 0 1555 (06.0.3) Volume--volume change > wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) Volume nonvolatile content volume nonvolatile matter in clear/pigmented coatings, test, 02697 (06.01) Volume solids d calculating formulation physical constants of paints/coatings, practice, D5201 (06.01) Volumetric measurement water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, 0 4942 (06.01) , Washability interior architectural coatings, test, D 3450 (06.01) practical washability of organic coatings, test, 0 4828 (06.01) Water water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, 0 4942 (06.01) Water--high-purity/reagent-grade reagent water, spec., 01193 (06.03) Water--resistance See Resistance--water Water--sea water erosion testing of antifouling paints, using high velocity water, test, D 4938 (06.01) organotin release rates of antifbuling coating systems in sea water, using graphite furnace atomic absorption spectrophotometry (GF-AAS), test, 0 5108 (06.01) subjecting marine antifouling coating to bifouling and flirii shear forces iri natural seawater,, test, D 4939 (06.01) Water absorption comparative corrosion preventive characteristics of materials used for joints/couplings/fittings/patches in pipeline coatings, test, G18 (06.01) water penetration into pipeline coatings, test, G 9 (06.01) Water-base paints See Latex paints Water channel method erosion testing of antifoulingpaints, using high velocity water, test, D4938 (06.01) Watercolor paint Sa Artists' paints artists' watercolor paints, spec.,, I>.5p67 (06.01) Water content--paints/relatedcoatings/materials f cresylic acid content (of alkaline cresylate solutions), chemical analysis, 03439 (06.03) fatty nitrogen compounds, test^D 2072 (06.03) Karl Fischer reagent method, test, D 4017 (06.01) moisture content of pigments, 0 1208 (06.02) oil/wafer presence in compressed air (used for coating application/air blast cleaning/abrasive blast cleaning), 04285(06.01) phenol/related materials, by iodine'reagent method, test, D 1631 (06.03) water content of water-reducible paints, by direct injection into gas chromatograph, test, 0 3792 (06.01) water in liquid naval stores, tes't. D 890 (06.03) water in volatile sqlvents, by Fischer reagent titration method, test, D1364 (06.03) Water content--petroleum products water in petroleum pioducts/bituminous materials, by distillation^ test, 0 95 (O6'.0i, 06.03) Water fog test , . testing water resistance of coatings, using water fog apparatus, practice, D1735 (06.01) Water immersion resistance to failure of paints, and related coatings, on steel surfaces, 0870 (06.01); Water-insoluble impurities content See Impurities (headings) Water-insoluble matter content ' ' apparent pH of water insoluble phenol-formaldehyde rdsin, test, D 4613 (06.02) hydrogen sulfide/sulfur dioxide (quantitative) of industrial aromatic hydrocarbons, test/D 2363 (06.02) -- methylcellulose, test, 0 1347 (06.02) ' Water miscibility *-- Sa Miscibility ;' water miscibility of water-soluble solvents, test, 0 1722 (06.03) Water of hydration calcium borosilicate, test, D 4487 (06.02) Water penetration water penetration into pipeline coatings, test, G 9 (06.01) Water pickup water pickup of lithographic printing inks/vehicles in a laboratory mixer, test, 0 4942 (06.01) Water-reducible coatings testing industrial water-reducible coatings, guide, D 4712 (06.01) Water repellency wood products, qualitative test for, D 2921 (06.01) Water resistance See: Resistance--water Water-solublermatter content conductimetric analysis of water-soluble ionic contamination of blasting abrasives, test, 0 4940 (06.01) moisture content of pigments, D 1208 (06,02) painting inspectors (metal substrates), guide, 0 3276 (06.01) 1196 Vi DU P050298372 Index of ASTM Standards, Section 6 Wijs procedure--iodine value salt content ofblue pigments, test, D 1135 (06.02) sampling/testing lac resins (orange shellac/button lac/gamet lac/bleached lac), test, 0 29 (06.02) water miscibility of water-soluble solvents, test, D1722 (06.03) water-soluble salts in pigments* jjy measuring specific resistance of pigment leachate, test, 1> 2448 (06i02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, 0 126 (06.02) Water-soluble solvents < See Solvents [headings). Water spotting reporting paint film fhilures characteristic of exterior latex paints, classification, D 1848 (06.01) Water vapor permeance moisture vapor transmission of organic coating films, ,test, D 1653 (06.01) . ... Water vapor transmission moisture vapor transmission of organic coating films, test, D 1653 (06.01) Waxes alcohol-benzene soluble matter, in cellulose, test, 01794 (06.02) Wear testing resistance to wear of traffic paint, method, A D 913 (06.01) Weathering conducting tests on paint/vamish/lacquer/relaled products, using enclosed carbon-arc light/water exposure apparatus, practice, D 5031 (06.01) evaluation, of painted/coated specimens subjected to corrosive enviromrients. fhethSd, 01654 (06.01) panel, recording,results of exposure tests, singfe-/multi-panel forms, A 01150 (06.01) Weathering--accelerated and outdoor accelerated testing ofpaihts/varcishes/lacquers/related products, using filtered open flame, carbon-arc Ught/water exposure apparatus, practice, D 822 (06.01) ' coatiiigl(applied to metal substrates), practice, 04141 (06.01) Dew cycle, light-water-exposure apparatus, practice for operating, 0 3361 (06.01) ', testing water resistance of coatings, using water fog apparatus, practice, 01735 (06.01) ' Weathering--outdoor conducting ijxterior exposure tests of (exterior) paints on steel, test, D1014 (06.01) conducting exterior exposure tests of house/trim paints on , : new/unpainted wood, practice, D 1006 (06,01) . , , effects of outdoor weathering on pipeline coatings, test, Gil (06.01) , . , ,;n exposure of paints/related coatings to fluorescent UY<- cSndensatiop light-water-expospre apparatus, practice for conducting tests, 0 4587 (06.01) quantifying dirt collection on coated exterior panels, test, D 3719 (06.01) /, wood used as panels iii weathering tests of coatings, spec.,' D358 (06.01) Weight impact resistance of pipeline coatings, by falling weightiest,! G 14 (06.01) paint/vamish/lacquer/related products, test, A D1475 (06.01) transfer efficiency under production conditions for spray application of automotive paints, by weight basis, practice, D 5066 (06.01) volume/weight of industrial ardmatic hydrocarbons, method, D 1555 (06.03) Weight--weight loss wet abrasion resistance of interior paints to scrubbing, by weight loss, test, D 4213 (06.01) : Weight--weight-per-gallon cup paint/vamish/laeqflpE/related products, test, A D 1475 (06,01) Weight percent epoxide (WPE) > epoxy content Ofepoxy.resins, test, D 1652 (06.02) Weight solids ' calculating formulation physical constants of paints/coatings, practice, D 5201 (06.01) Weissenberg rheogoniometer test viscosity of polymeric powders and powder coatings, practice, D 3451 (06.01) Welding/welds design/fabrication of flue gas desulfurization system components (for protective lining application), spec., 04618 (06.01) Western red cedar ' wood used as panels in weathering tests of coatings, spec,, 0358(06.01) Wet film thicbitess See Film--wet film thickness Wet film thickness gage wet film thickness of Organic coatings, 01212 (06.01) Wet grouiidf inuscovite mica See Stone--mica Wet-to-dry hiding change wet-to-dry hiding change of architectural coatings, test, 0 5007(06.01) White architectural enamels See Architectural coatings White ( `Hie See Extender pigments White hiding pigments See Antimony oxide/Basic carbonate white lead Sa Basic sulfate white lead/Lea'ded zinc oxide Pigments (general pfoperties)/Titaninm dioxide Zinc oxide/Zinc sulfide White linseed-oil paints white linseed oil paints- chemical .analysis, selecting test methods, practice, D 215 (06.01) White pigments--general analysis analysis of white zinc pigments, test, 0 3280 (06.02) antimony oxide content of white pigment (separated from solvent-type paints), test, 0 2350 (06.02) basic carbonate white lead pigment, spec., 0 81 (06.02) chemical analysis of white pigments, selection of test methods, guide, 0 34 (06.02) particle size distribution, by hydrometer of common white extender pigments, test, 0 3360 (06.02) ratio of anatase to rutile in titanium dioxide (Ti02) pigments, by x-ray diffraction, test, 0 3720 (06.02) relative tinting strength of white pigments, by reflectance measurements, test, 0 2745 (06.02) relative tinting strength of white pigments, by visual observation, test, 0 332 (06.02) . _ __ sulfide in white pigment separated from solvent-reducible paints, test, 0 2351 (06:02) 'sulfur dibxide in white piflineht Separated from solventreducible paints, test, 0 2352 (06.02) white lead- chemical analysis, test, 0 1301 (06.02) white linseed oil paints- chemical analysis, selecting test methods, practice, 0 215 (06.01) white titanium pigments, chemical analysis, test, D1394 (06.02) zinc oxide pigments, spec:, 0 79 (06.02) White pine wood used aS: panels in weathering tests ofcoatings, spec., 0358(064)1) White zinc pigments See Zinc oxide Whiting See Calcium carbonate Wick test sustained burning (of low viscosity liquid mixtures), by Wick test, 0 4207 (06.03) Wijs procedure--iodine value drying oils and their derivatives, test, 0 1959 (06.03) 1197 DUP050298373 Wijs procedure--iodine value Index of ASTM Standards, Section 6 fatty amines/diamines, test, D 2075 (06.03) Wire-wound drawdown bar method coil coatings, application using a wire-wound drawdown'bar, practice, D4147 (06.01) Wolfe-potentiometric method oleic acid content of tall oil rosin, test, D1585 (06.03) Wood and wood products chlorinated phenol;preservative content in wood products, qualitative test, D 2921 (06.01). temperature of applied coatings on wood products during the curing cycle, by infrared radiation thermometers, practice, 17 3259 (06.01) < wood used as panels in weathering tests of coatings;spec., 1)358(06.01) i Wood and wood products--cellulose pulp metals (iron/copper/manganese/calcmm) content of cellulose pulp (from wood/cotton), by atomic spectrophotometry,, * test, D 4085 (06.02) ; pentosans content of cellulose, test, D1787 (06.02) Wood and wood products--composites edge performance of composite wood products under surfactant accelerated moisture stress, test, D 2065 (06.01) Wood and wood products--heartwood wood used as panels in weathering tests of coatings, spec., D 358 (06.01) Wood and wood products--paints/related coatings, block resistance of organic coatings, test, 0 2793 (06,01) conducting bxterior exposure tests of house/tipii; paints on new/unpainted wood, practice, tb 1006 (06.01) dry film thickness, by microscopical measurement, D 2691 (06.01) factory-primed, durability and compatibility, with finish coatings, test, D 2830 (06.01) humid-dry cycling (for coatings on wood/wood products), method, D 3459 (06.01) :, specifying properties of paint from the liquid-state through the curing stage for factory applied coatings on wood products, practices, D 2336 (06-01) - Wood preservatives - chlorinated phenol preservative content in wood products, qualitative test, D 2921 (06D1) ` " Wood rosin ;. See Rosin Sa Oils (headings) ,' Wood turpentine See Turpentine x :: : Xenon lamps lightfastness ofpigments (in artists' paints), test, D 4303 (06,01) operating light-exposure apparatus (Xenon-arc type) doth/ ; ' without water for exposure of nonmetallic materials, practice, G 26 (06.01) ` X-ray diffraction , ratio of anatase to rutile in titanium dioxide (Tib*) pigments, by x-ray diffraction, test, D 3720 (06.02) Xylene acidity of benzene/toluene/xylenes/solvent r.aphthas/similar industrial aromatic hydrocarbons, test, D 847 (06.03) acid wash color, test, 0 848 (06.03) aromatic hydrocarbons/related chemicals, terminology, 0 4790(06.03) distillation, test, D 850 (06.03) fiash/fire point of liquids, by Tag open-cup apparatus, test, D1310 (06.03) impurities in high-purity ethylbenzene, by gas chromatography, test, D 5060 (06.03) purity of hydrocarbons from freezing points, test, D 1016 (06.03) sampfing/handling liquid cyclic products (at ambient temperature), practice/D 3437 (06.03) total non-aromatic/trace monocyclic hydrocarbon aromatic hydrocarbons in high-purity benzene/toluene/mixed zylenes, by gas chromatography, test, D2360 (06.03) volume/weight of itidt&ial aromatic hydrocarbons, method, D1555 (06.03) xylene isomer analysis, by gas chromatography, test,' D 2306 (06.03) xylenes for p-xylene feedstock, spec., D 5211 (06.03) meta-Xylene apparent density ofindustrial'aromatic hydrocarbons, test, 02935(06.03) commercial density (of pure liquid chemicals), test, ' D 3505 (06.03) volume/weight of industrial aromatic hydrocarbons, method, D1555 (06.03) ort/to-Xylehe apparent density of industrial aromatic hydrocarbons, test, D 2935 (0603) commercial density (of pure liquid chemicals), test,: 0 3505(06.03) purity,- by gas chromatography, test, D 3797 (06.03) volume/weight of industrial arpinalic hydrocarbons, method, 0 1555(0603) o-xylene 950, spec., D 4076 (06.03) para-Xylene .. analysis ct'p-xykSofy by gas chrSfedtOgraphy, method, 0 3798(06.03) apparent density 6f industrial afoihatie hydrocarbons, test, 0 2935 (06.03) commercial density (of pure liquid chemicals), test, 03505(06.03) highjiurityp-xylene, spec., D,5136 (06.03) trace (total) chloride (organic/inorganic) in liquid aromatic hydrocarbons, test, D 5194 (06'.03) volume/weight of industrial aromatic hydrocarbons, method, 0 1555 (06.03) xylenes for p-xylene feedstock, spec., 0 5211 (06.03) Xylene (five-degree) xylene isomer analysis* by gas chromatography, test, 0 2306 (06.03) Xylene (mixed) apparent density of industrial aromatic hydrocarbons, test, 02935(06.03) < commercial density (of pure liquid chemicals); test, 0 3505(06.03) ! >: volume/vi/eight ofindustriaT'hroinattf hydrocarbons, method, D1555 (06.03) Xylene (nitration grade) xylene isomer analysis, by. gas chromatography, test, D 2306 (06.03) xylene (nitration grade), spec., 0 843 (06.03) Xylene (ten-degree) xylene isomer analysis, by gas chromatography, test, . D 2306 (06.03) Xylenol . water content, by iodine reagent method, test, 01631 (06.03) Y Yellow ocher See Ocher Yellow pigments chrome yellow/orange pigment, spec., 0211 (06.02) yellow iron oxide (hydrated), spec., D 768 (06.02) yellow/orange/green pigments containing lead chromate/ chromium oxide green, analysis, test, D126 (06.02) Index of ASTM Standards, Section 6 Yield value laboratory preparation of gelled vehicles, using microwave oven, practice, D 5166 (06.02) z Zahn viscometers See Viscometers--Zahn Zeisel technique ethoxy] substitution in cellulose ether products, by gas chromatography, test, D 4794 (06.02) gas chromatographic analysis of methoxyl/hydroxypropyl substitution, in cellulose ether products, test, D 3876 (06.02) Zinc liquid paint driers, selection of test methods, D 564 (06.03) Zinc chromate (yellow) analysis, D 444 (06.02) zinc yellow (zinc chromate) pigments, spec., D 478 (06.02) Zinc-coated (galvanized) surfaces preparation for painting, practice, D 2092 (06.01) Zinc content analysis of white zinc pigments, test, D 3280 (06.02) paint driers, by EDTA method, test, D 2613 (06.03) zinc dust (metallic zinc powder), test, D 521 (06.02) zinc yellow (zinc chromate yellow) pigment, test, D 444 (06.02) Zinc driers See Driers ZTO chromate Sa Oils--drying Zinc dust Sa Pigments (general properties) analysis, D 521 (06.02) zinc dust pigment, spec., D 520 (06.02) Zinc hydroxy phosphite analysis, D 4450 (06.02) zinc hydroxy phosphite pigment, spec., D 4462 (06.02) Zinc oxide--pigment analysis of white zinc pigments, test, D 3280 (06.02) zinc oxide pigments, spec., D 79 (06.02) Zinc oxide content zinc hydroxy phosphite, test, D 4450 (06.02) Zinc-rich primer Sa Primer MEK resistance of ethyl silicate (inorganic) zinc-rich primers, by solvent rub, test, D 4752 (06.01) Zinc snliide analysis of white zinc pigments, test, D 3280 (06.02) Zinc white See Zinc oxide--pigment Zinc yellow , See Zinc chromate (yellow) Zirconium content paint driers, by EDTA method, test, D 3969 (06.03) ZTO chromate See Zinc chromate (yellow) r r 1199 DUP05 02 98375 1916 Race Street Philadelphia, PA 19103 Phone: (2151 299-5454 FAX: 1215) 977-9679 European Office 27-29 Knowl Piece, WiJbury Way Hitchin, Herts SG4 OSX, England Phone: 0462-437933 FAX: 0462-433678 THIS APPLICATION IS FOR SOCIETY MEMBERSHIP ONLY. 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